3025BOLEAD BATTERY SITE

TREATABILITY STUDIES

byPEI Associates, Inc.Cincinnati, Ohio 45246

Contract No. 68-03*3413Work Assignment No. 1-19, Tasks G, K, and 0

Technical Project MonitorMr. Richard P, Traver, P.E.Releases Control Branch

Risk Reduction Engineering LaboratoryEdison. New Jersey 08837

RISK REDUCTION ENGINEERING LABORATORYOFFICE OF RESEARCH AND DEVELOPMENTU.S. ENVIRONMENTAL PROTECTION AGENCY

CINCINNATI. OHIO 45268

302561

DISCLAIMER

The Information In this document has been funded wholly or In part bythe United States Environmental Protection Agency under Contract No.68-03-3413, Work Assignment No. 1-19, Task J, to PEI Associates, Inc. It hasbeen subjected to the Agency's peer and administrative review, and It hasbeen approved for publication as an EPA document. Mention of trade names orcommercial products does not constitute endorsement or recommendation foruse.

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302582FOREWORD

i*

Today's rapidly .developing and changing technologies and industrialproducts and practices frequently carry with them the Increased generation ofmaterials that, If improperly dealt with, can threaten both public healthand the environment. The U.S. Environmental Protection Agency 1s charged byCongress with protecting the Nation's land, air, and water resources. Undera mandate of national environmental laws, the Agency strives to formulate andImplement actions leading to a compatible balance between human activitiesand the ability of natural systems to support and nurture life. These lawsdirect the ERA to perform research to define our environmental problems,measure the Impacts* and search for solutions.

The Risk Reduction Engineering Laboratory Is responsible for planning,implementing, and managing research, development, and demonstration programsto provide an authoritative, defensible engineering basis in support of thepolicies, programs, and regulations of the EPA with respect to drinkingwater, wastewater, pesticides, toxic substances, solid and hazardous wastes,and Superfund-related activities. This publication is one of the products ofthat research and provides a vital communication link between the researcherand the user community.

This document describes the methodology and results of bench-scale soilwashing and stabilization/solidification treatability studies conducted ohcontaminated toil and debris from six Superfund sites. Specifically, lead-contaminated soil and debris from past metal-recycling operations was subjectto soil washing with aqueous solutions of chelate and surfactant. Selectedresiduals were further treated by solidification/stabilization* The resultsof this stuo> can be used by Regional Remedial Project Managers, EPA contrac-tors, and responsible parties for determining the feasibility of utilizingsoil washing and stabilization/solidification in the cleanup of lead-contami-nated soil and debris.

E. Timothy Oppelt, DirectorRisk Reduction Engineering Laboratory

302583

ABSTRACT

In 1984, Congress passed the Hazardous and Solid Waste Amendments (HSWA)to the Resource Conservation and Recovery Act (RCRA) to minimize the volumeof hazardous and toxic wastes deposited In permitted hazardous waste landfills.This legislation urged the development of new technologies and cleanup pro- .cedures for the treatment of contaminated waste material found at SuperfundSites before its final disposal. The focus of this study was to determinethe feasibility of using soil washing and/or stabilization/solidification toreduce lead contamination at the following six metals-recycling Superfundsites; 1) Old Man's Township, Salem County, New Jersey; 2) CftR Battery Co.,Inc., Chersterfleld County, Virginia; 3} Schuylkill Metals Corp., Plant City,Florida; 4) fiould, Inc., Portland, Oregon} 5) J&L Fabricating, Leeds,Alabama; and 6) Passes Chemical Co., Fort Worth, Texas. Bench-scale tollwashing studies using water, a surfactant solution, and a chelate solutionwere conducted on the contaminated soil and debris frorr these Superfundsites. The experiments entailed mixing the soil With the wash solution on areciprocating shaker, wet-iltving the washed soil Into three size fractions(>2 inn, 0,25 to I mm, and <0.25 mm), and filtering the wash solution. Theresidual fines from the Gould site were treated further with stabilization/solidification techniques. The raw coil, treated soil fractions, and spentwash waters were analyzed for total lead and EP Toxlclty lead.

This report was submitted 1n fulfillment of Contract No. 68-03-3413,Work Assignment No. 2-19, PN 3741-I9-1J, by PEI Associates, Inc., Cincinnati,Ohio 45246 under the sponsorship of the U.S. Environmental Protection Agency.

1v

302581*CONTENTS

Foreword 111Abstract 1vFigures v1Tables v111Acknowledgement x

1. Introduction 1-11.1 Background 1-11.2 Objectives and scope 1-21.3 Site profiles 1-4

2* Conclusions and Recommendations 2-12.1 Conclusions 2-12.2 Recommendations 2-3

3, Experimental Design and Procedures 3-13.1 Sample acquisition and characterization 3-13.2 Test plan 3-33.3 Experimental procedures 3-33.4 Sampling and analysis 3-8

4. Bureau of Mines Approach 4-14,1 Bureau of Mines leach-electrolytic technology 4-24.2 Comparison of Bureau of Mines and PEI tr«atab1Hty studies 4-9

5. Results and Discussion 5-15.1 Sample characterization 5-15.2 Soil washing tests 5-45.3 Stabilization/solidification 5-355.4 Quality assurance 5-36

AppendicesA Standard Operating Procedures A-lB Soil Characterization Data B-lC Results of Soil Washing C*l

302585

FIGURES

Number Page1-1 Locations of Battery-Recycling Sites 1-33-1 Overall Test Plan 3-43-2 Proposed Soil Washing Procedure 3-63-3 Battery Casing Washing Procedure 3-73-4 Solidification and Stabilization Studies 3-94-1 Bureau of Mines Electrolytic Process for Recovering Lead

From Battery Scrap 4-34-2 Bureau of Mines Conceptual Process for Treating Battery

Breaker Residue 4-7 *•••»4-3 Bureau of Mines Conceptual Process for Treating Lead-

. Contaminated Soil 4-95-1 Old Man's Township: Total Pb Concentrations In Washed

Soil Fractions 5-75-2 C&R: Total Pb Concentrations 1n Washed Soil Fractions 5-75-3 Schuylklll: Total Pb Concentrations In Washed Soil

Fractions 5-85-4 Gould Soil; Total Pb Concentrations 1n Washed Soil

Fractions 5-85-5 Gould Casings; Total Pb Concentrations In Washed Soil

Fractions 5-95-6 J&L Fabricating: Total Pb Concentrations In Washed

Soil Fractions . 5*95-7 Penes: Total Pb Concentrations In Washed Soil Fractions 5-11

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302587

TABLES

Number Page

3-1 List of Soils Characterization Analytical Parameters 3-23-2 Analytical Matrix 3-104*1 Bureau of Mines Data for Washing Battery Casings 4-44-2 Results of Cleaning Battery Casings In 5 Percent EDTA

Solution 4-54-3 Results of Sludge Leaching Tests 4*54-4 Solubility of Lead Compounds 1n EDTA 4-64-5 Summary of Preliminary Results From Soil Washing of

United Scrap Lead Soil 4-85-1 Sample Characterization 5-25-2 Distribution of Soil Collected 1n Each Fraction 5-55-3 Pb Concentrations in Soils Fractions and Filtrates 5-65-4 Pb, Cd, N1, and Cu Concentrations 1n Soil Fractions ana

Liquid Filtrates for Pesses Soil 5-105-5 Percentage Reduction of Lead Concentrations From the

Untreated Soil 5-135-6 Percentage Reduction of Metal Concentrations From the

Untreated Pemt Soil 5*145-7 Percent of Lead 1n Untreated Soil Recovered 1n Wash

Filtrate and Soil Fractions 5-165-8 Percent of Metal Contaminants In Pesses Soil Recovered

In Liquid Filtrates and Soil Fractions 5-20

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302588TABLES (continued)

Number Page

5-9 Percentage Removals of Total Lead as Compared WithControl {Water Wash) 5-24

5-10 Pesses: Percentage Removals of Total Metals as Compared'With Control (Water Wash) S-25

5-11 Percentage of Lead Recovered In Wash Solution 5-265-12 Percentage of Metals Recovered 1n Wash Solution for the

Pesses Site 5-26

5-13 Lead CheUtlng Efficiency of EDTA 5-28

5-14 Lead CheUting Efficiency of EDTA on the Pesses Soil 5-29

5-15 TCLP Lead for the Gould Soil 5-31

5-16 TCLP Lead on Soil Fractions Washed with EDTA 5-315-17 TCLP Lead for the J&L Fabricating Soil 5-32

5-18 EP Toxicity Lead for the J&L Fabricating Soil S-32

5-19 TCLP Metals for the Pesses Soil 5-33

5-20 EP Toxicity Metals for the Pesses Soil 5-34

5-21 Characterization of the Goufd F1nes"After Washing 5-35

5-22 Results of Stabilization/Solidification of the SoilWashing Residual From the SouTd Site 5-37

5-23 QA/QC Results for Soil Washing 5-3B

5-24 Relative Percent Difference for Duplicate Runs 5-39

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302589

ACKNOWLEDGEMENT

This report was prepared for the U.S. Environmental Protection Agency,Office of Research and Development, Risk Reduction Engineering Laboratory,Cincinnati, Ohio, by PEI Associates, Inc., under Contract No. 68-03-3413.Mr. Richard P. Traver served as the EPA Technical Project Monitor. Ms, JudyL. Hessling was PEI's Work Assignment Manager, Messrs. Jeffrey Davis andSteve GUI-Pour were the principal investigators, Ms. Barbara B. Locke wasthe Senior Reviewer,

The authors gratefully acknowledge Dr. Richard Snow and his staff (IITResearch Institute) for their assistance 1n conducting the soil washingstudies; Mr* Richard McCandless and his staff (University of Cincinnati) forconducting the stabilization studies; the Regional RPMs for coordinating thesample acquisition; Ms. Pat Esposito (Bruck, Hartman & Esposito, Inc.) forher assistance in analyzing and interpreting the data and writing the report;and Dr. David Leggett (Dow Chemical USA) for his Instruction on chelationchemistry.

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302590

SECTION 1

INTRODUCTION

LI BACKGROUND

Under the Comprehensive Environmental Response, Compensation, and Liabil-ity Act (CERCLA} and the National Contingency Plan that Implements it, re-sponse actions at hazardous waste sites must reduce the threat of uncon*trolled contamination resulting from the treatment, storage, or disposal ofhazardous compounds. Until recent years, this has often meant the excavationand removal of contaminated material from uncontrolled sites and its subse-quent disposal in permitted landfills. In 1984, Congress passed the Hazard-ous and Solid Waste Amendments (HSWA) to the Resource Conservation andRecovery Act (RCRA) to minimize the volume of such wastes deposited in per-mitted hazardous waste landfills. This legislation urged the development ofnew technologies and cleanup procedures for the treatment of contaminatedwaste material found at CERCLA Sites before its final disposal.

This statute requires the U.S* Environmental Protection Agency (EPA)Office of Solid Waste and Emergency Response to discourage containment-baseddisposal of CERCLA wastes and to encourage the establishment of levels ormethods of treatment that will substantially diminish the toxicity of thewaste or significantly reduce the likelihood of migration of hazardousconstituents from the waste and thereby minimize short-term and long-termthreats to human health and the environment. As landfill space becomes morelimited and expensive and control of the transportation of the waste materialbecomes more stringent, onslte treatment will become more economical, safe,and desirable if the waste material can be handled by the application ofsound and we11-developed technologies.

Soil and debris contaminated by lead (Pb) and other heavy metals, suchas cadmium (Cd), copper (Cu), and nickel (Ni), present problems at manyhazardous waste sites where metals recycling and reclamation activities havebeen conducted. Typical examples are sites where used batteries arecollected and processed by various cracking and secondary smelting opera-tions. Piles of spent battery casings as well as slag and dust from furnaceoperations are often found at such sites. At these sites, soil contaminationby metals can typically reach levels in the hundreds and thousands of partsper million (milligrams per kilogram). At some sites, lead levels as high as10 percent have been found in the soil. Twenty-three battery-recycling sitescurrently appear on the United States' priority listing of contaminated sitesrequiring cleanup under CERCLA, and many others are known to exist that arenot yet on the priority list for remediation.

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1.2 OBJECTIVES AND SCOPE 30^591

The focus of this study was to determine the feasibility of using soilwashing and/or stabilization/solidification to reduce lead contamination atthe following six metals-recycling Superfund Sites:

1) Old Man's Township, Salem County, New Jersey, Region II.

2} C&R Battery Co., Inc., Chesterfield County, Virginia, Region III.

3) Schuylkill Metals Corp., Plant City, Florida, Region IV.4) Gould, Inc., Portland, Oregon, Region X.

5) J&L Fabricating, Leeds, Alabama, Region IV,6} Pesses Chemical Co., Fort Worth, Texas, Region VI.

Figure 1-1 shows the location of each of these sites. The sites areformer lead battery reclamation facilities (except the Pesses site, which wasused as a metals-recycling facility for the recovery of nickel and cadmiumfrom nickel-cadmium batteries) that have been proposed or listed on theSuperfund National Properties List (NPL), The primary waste materials atthese sites are broken battery casings [consisting of hard rubber (ebonite)and plastic] and soils contaminated with lead. At the J&L Fabricating andPesses sites, analyses of the soil samples indicated the presence of thefollowing contaminants in addition to lead: heavy metals such as nickel andchromium at J&L Fabricating; and copper, nickel, and cadmium at Pesses,

Regions IIf III, IV, VI, and X have requested EPA's Office of Researchand Development-Risk Redaction Engineering Laboratory (ORD-RREL) to assistthem in evaluating the feasibility of using a soil washing/volume reductiontechnology followed by stabilization/solidification for the remediation ofthe contaminated soils at these sites. In addition, soil washing was alsotested on the Gould rubber battery casings. Therefore, the purpose of thisstudy can be sunmarized as follows:

* To evaluate soil washing as a treatment technology for lead-contaminated soils and battery casings.

s To Identify contaminants and soil characteristics affectingtreatment efficiency.

° To study the partitioning of metals relative to soil particlesizes.

0 To evaluate stabilization/solidification of selected residuals fromsoil washing that fail EP Toxicity tests for lead.

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To evaluate the soil washing technique, the soil samples from thesesites were subjected to a bench-scale washing cycle with water, a cheatingagent (EDTA). or-a surfactant (Tide). After a 30-minute contact period, thesoils were removed from the washing solution and separated into three dis-tinct size fractions during the rinsing operation to study the partitioningof metals relative to particle size. At the Gould site only, PEI alsoevaluated solidification/stabilization (S/S) of the raw soil and residualsoil fractions (less than 2 mm) from the soil washing tests.

In addition to the soil washing and stabilization/solidification evalua-tions performed, PEI had originally proposed to investigate a leaching pro-cess developed by the U.S. Bureau of Mines. This process uses fluosilicicacid to leach lead from contaminated soil and debris. Because of time andbudgetary constraints, PEI was unable to evaluate this process; however,Section 4 of this report provides more detail on the Bureau leaching processso the reader can become familiar with this process and perhaps investigateits ability to reduce lead (and possibly other metal) concentrations incontaminated soil and debris.

Other sections of this report present an analysis of the results of thesoil washing and S/S bench-scale studies actually conducted. The backgroundoperations and geophysical properties of the soil end contaminant levels ateach site are also described in detail, and the experimental bench-scaleprocedures are explained.

1.3 SITE PROFILES

The six sites addressed in this study are among the highest prioritysites for cleanup under CERCLA. As shown in Figure 1-1, these sites repre-sent a broad range of geographic locations, climatological conditions, andnative soil types. A variety of process operations and waste disposal prac-tices over many years contributed to soil contamination at these sites.Detailed information on each site is presented in the following subsections.

Old Man's TownshipThis Superfund Site is located in Old Man's Township, Salem County, New

Jersey* Automotive battery-recycling and secondary lead smelting and re-fining operations at this 46-acre site began In 1972 and continued for 12years, Recycling operations consisted of cracking the batteries, drainingthe acid, removing the lead plates, and crushing the casings. The scrap leanwas then smelted in a blast furnace or (later) a rotary kiln and refined toproduce soft lead or antimonial lead. Furnace gases passed through an 18-cell fabric filter system for particulate removal. Lead-bearing wastes,including the crushed battery casings (rubber and plastic), blast furnace andkiln slag, and fabric filter dust, were piled, buried, or landfilled on site.In 1980, the owner entered into an Administrative Consent Order to remediatesoil and ground-water contamination at the site; in 1983, the site was listedon the Superfund National Priorities List (NPL). The interim remedial

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investigation/feasibility study report (Oanuary 1989) indicates that soils Inthe plant area contain lead concentrations up to 12,700 mg/kg of soil;samples tested by PEI contained lead concentrations up to 60,500 mg/kg,Current activities on site are associated with closure and post-closure careof the landfill. The State of New Jersey has set a cleanup standard of250-1000 ppm total lead for this site.

CiR Battery Co,The C&R Battery Co., Inc., Superfund Site is located in Chesterfield

County, Virginia* Lead-acid batteries were recycled at this 4,5-acre sitefrom the early 1970's until 1985. Lead and lead compounds were removed fromthe batteries and shipped offsite for processing. Acid was drained Intoonsite lagoons, and broken battery casings (primarily plastic) were shreddedand stockpiled on site* During a 1986 removal action, acidic liquids werepumped from the lagoons* neutralized, and discharged to a storm sewer; sludgewas excavated, blended with hydrated lime, and returned to the lagoon; andsurface soils were disked with lime to a depth of 2 ft. An 800-ft8 mound ofsoil mixed with battery casings remains on the site. Lead concentrations ashigh as 67,700 mg/kg have been previously measured in-the soil; samplestested by PEI contained lead concentrations as high as 82,800 mg/kg; elevatedlevels of arsenic* cadmium, copper, nickel, and 2inc have also been detected.As of September 1989, no cleanup standard had been set for this site.

Schuylkill Metals Corp.The Schuylkill Metals Corp. Superfund Site is located in Plant City,

Florida. From 1972 to 1986, a lead-acid battery reclamation facility wasoperated on this 17,4-acre site. Lead and lead oxide were removed from dis-carded batteries and shipped offsite for suiting. Initially, rubber batterycasings were crushed and used as fill and paving near the processing area;several tons of this fill material was later excavated for recovery of addi-tional lead* Plastic casings, which eventually replaced rubber in the manu-facture of batteries, were crushed and sold to a recycler. Until 1981, sul-furic acid from the discarded batteries was treated with lime (calcium oxide)or ammonia and discharged to a 22-acre unlined holding pond; in later years,the wastewater was neutralized and discharged under permit to a publiclyowned treatment works (PQTW). Some waste acid also was marketed to thephosphate industry as a processing agent. Lead concentrations in the pondsediments are generally below 500 mg/kg, but they range up to 40,000 mg/kg inthe process area soils. A cleanup standard of 500 to 530 ppm total lead hasbeen designated for this site.

GouldThe Sould, Inc., Superfund Site is located in Portland, Oregon. This

Pacific Northwest site covers approximately 60 acres in a heavily industria-lized area. Battery recycling, secondary lead smelting and refining, zincalloying and casting, and cable sweating operations began in 1949; lead oxideproduction began In 1965, Over the 30-year operating life of the facility,86,900 tons of waste battery casings (rubber and plastic), 119800 tons ofmatte (composed of iron and lead sulfides), and 6.57 million gallons of

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302595sulfuHc acid were disposed of on the site and adjacent property* Approxi-mately 98 percent of the battery casings are burled below the surface, wherethey are in direct contact with the ground water. Concentrations of lead 1nthe battery casing wastes range up to 190,000 mg/kg; concentrations of leadin the surrounding surface soils range up to 20,000 mg/kg. Samples tested byPEI contained lead concentrations up to 288,000 mg/kg for the battery cas-ings, and 29,500 mg/kg for the soil. An estimated 22,000 yd3 of soil re-quires treatment by removal. The site was listed on the NPL 1n 1983. Thereare two cleanup standards currently in effect for this site; soils below thesurface must be cleaned to 5 ppm EP Toxicity and soils at the surface mustshow levels below 1000 ppm total lead.

J&L FabricatingThe 1LCO Superfund Site 1n Leeds, Alabama, consists of several parcels

of land where lead-bearing wastes from the main ILCO lead-acid battery-recycling and secondary smelting facility were deposited as fill. The soilsused in this study were obtained from the parcel of land owned by J&LFabricating and will be referred to as such in this report. Operations atthe facility involved battery cracking and separation of lead-bearing solids,followed by lead smelting, refining, alloying, and casting. Waste acid andrubber and plastic chips from the battery-cracking operation were shippedoffsite for recycling or disposal* Slag from the smelting/refining operationwas accumulated in waste piles on site. In 1986, the facility began addingcalcium sulfate sludge to the blast furnace slag to immobilize the lead; thefixed slag was then disposed of in the county landfill. Soil samplescollected from various locations during the 1987 remedial investigationindicate that lead contamination averages more than 1000 mg/kg over most ofthe site and exceeds 30,000 mg/kg in some areas.

Pesses Chemical Company

The Pesses Chemical Company Superfund Site 1s located in Fort Worth,Texas* From 1979 to 1981, a nickel-cadmium battery-recycling facilityoperated on this 6*7-acre site. The batteries were charged to one of fourfurnaces, and cadmium, which was driven off from the process as cadmiumoxide, was condensed from the exhaust gases and poured into molds. The moldswere then resmelted 1n a ball furnace, and the cadmium was recast into 1Mbballs for shipment to various plating operations. Furnace gases were ductedto the atmosphere. Cadmium emissions from the fabric filter, along withImproper storage and handling of process materials and residues, have contri-buted to widespread soil contamination at the site. Prior to an immediateremoval action in 1983, cadmium concentrations 1n the soil ranged up to 9000mg/kg. Although most of the contaminated materials and debris have now beenremoved, cadmium concentrations still range between 1000 and 5000 mg/kg overthe south portion of the site. Some concern regarding possible exposure ofneighboring residents to cadmium from fugitive dust emissions prompted thecapping of unpaved areas on the site. More recent sampling has shown thatthe soil 1s also contaminated with lead, copper, and nickel.

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302596

SECTION 2

CONCLUSIONS AND RECOMMENDATIONS

2,1 CONCLUSIONS

The following are the conclusions drawn from the data collection andevaluation effort described in the remainder of this report:

Q All sites except Gould are characterized by a carbonate soiljquartz and caldte (CaC03) are the primary minerals. Gould con-tains Na, Ca-feldspar instead of caldte. The Old Man's Townshipsoil is only slightly carbonated.

0 The presence of calcite signifies the presence of a carbonated formof lead, such as PbC03, Pbg(C03}a(OH}?, or PbitS0lt(C03)2(OH}£. Thepredominant lead forms 1n the Gould soil and battery casings arelead sulfate and lead dioxide, which result from the large amountsof battery waste still present on site. Battery casing samples arethe most acidic because of the sulfate content.

8 Soil washing did not remove significant amounts of lead from any ofthe soil fractions. Lead concentrations were not consistentlyhigher in any of the soil fractions, nor were they significantlydifferent among wash solutions, including water. When the waterwash reduced the lead concentration for a particular soil fraction,the surfactant and EDTA also reduced the lead concentrations, whichsignifies that mechanical agitation is a more important variablethan the wash solution used. In some soil fractions, concentra-tions appeared to increase after washing, possibly because ofvariability in the soil and the resulting difficulty in obtainingrepresentative samples. In the case of the Old Man's Townshipsoil, the clay particles formed a thick coating around the gravelparticles that were not removed during washing.

0 Lead in the soil was distributed among the soil fractions ratherthan being concentrated in the smaller particles,

0 A comparison of lead concentrations in the wash waters indicatedthe EDTA wash performed better than the surfactant and water. TheEDTA wash solubilized 13.8 to 23,5 percent of the lead in theuntreated soil. The higher the concentrations of EDTA, the higherthe concentrations of lead in solution were.

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0 Lead concentrations in the wash solution were higher in thesurfactant than in the water, which indicates that the surfactantsolubilized more lead. The surfactant solubilized 0,28 to 14,5percent of the lead in the untreated soil*

0 The surfactant worked equally well on the Gould battery casings andthe soil, but the EDTA worked significantly less well on thebattery casings.

0 The chelatlon efficiency was 3.6 to 7.5 percent for all soilsduring the second series of tests, and only 0*17 percent for theGould casings. The chelaticn efficiency during the first series oftests (on the O&L Fabricating soil) was significantly greater (13to 19 percent). Greater agitation during the first series of testsprobably produced a higher chelation efficiency,

0 Of the lead that was removed during washing, a large proportion wasalso leacha&le under the conditions of the TCLP. Lead concentra-tions in the TCLP extracts were significantly less than those inthe untreated soil; however, no soil fractions met the 5 rog/Lcriterion used to define a hazardous waste.

0 Results were not dependent an particle-size distribution, soilmineralogy, or lead speciation.

0 The quality assurance (QA) objectives were generally met for liquidsamples.

0 The QA objectives were not met for the precision and accuracy ofsolid samples because the variability of the samples made it diffi-cult to obtain a representative sample for analysis.

0 Lead concentrations on replicate test runs varied the most In thelarger particles and the least 1n the wash solutions and smallersoil fractions.

[Insert Stabilization/Solidification Results Here]

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3Q25982.2 RECOMMENDATIONS

The data collected during these experiments showed no significant reduc-tion in the total lead concentrations in the soil fractions, even though asignificant fraction of the lead was solubilized 1n the wash solution.Several procedural changes can be implemented to improve the chelation effi-ciency, lead solubillzation. experimental accuracy and precision, and confi-dence in the results. The following is a list of recommendations for proce-dural changes and future tests:

0 An Increase in the agitation of the solution 1s recommended to wetthe soil completely, to break up the larger particles, and to

. suspend the soil in the wash solution. This can be done byincreasing the vibration of the reciprocating shaker or by usingdifferent equipment, such as a ball mill or end-over-end extractionvessel.

0 The soil clumps in the untreated soil should be broken up prior towashing. Because the agitation was often insufficient to break upsuch clumps during current testing, the wash solution could notcome into contact with the Interior of the clumps. The clumps wereoften not broken up until the rinse phase. Over the years, thelead in the soil at the Superfund site may have migrated into theinterior of these clumps. Breaking up such clumps prior to washingwould increase the surface area exposed to the wash solution endenable more lead to be solubilized.

9 Extremely low filtration rates caused problems during the fieldtests of soil washing with EDTA, Use of larger filter size isrecommended to increase the filtration rate. In addition, the useof filtering aids to Improve the dewateHng characteristics andfiltering rate of wash solutions should be investigated,

0 The accuracy and precision of the experimental results could beincreased by additional homogenization of the untreated soil andthe different soil fractions, and by conducting more replicateanalyses. Sampling and analysis procedures should be carefullyconducted to increase the probability, of obtaining representativesamples.

0 Lack of adequate rinsing of the soil fractions after washing mayhave allowed soluble lead complexes to remain on the soil. Theprocedures should be revised to ensure adequate rinsing.

0 The work conducted by the Bureau of Mines should be tested by usingstandard soil washing procedures so that the resulting data wouldbe directly comparable to the data collected by PEI and others withdifferent wash solutions at various sites.

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0 - : If the bucfge't allows, "screening studies should be conducted underat least two conditions. The disadvantage of testing under onlyone set of conditions is that the resulting data can provide noindication of th'e effect of changing conditions on the overallperformance of the system. The data from the soil washing tests donot indicate definitely whether the system was at equilibrium orwhether different values for critical variables (agitation, reten-tion time, concentration of surfactant or chelate) would providebetter performance.

0 Different process trains need to be investigated, including thoseproposed by the Bureau of Mines. The current soil washing studiesexamine soil washing followed by solidification of the fines.Other possibilities include soil washing followed by fluosilicic ornitric acid leaching of the fines, or soil washing/leaching fol-lowed by selling the fines to a smelter. The soil fractions couldbe separated prior to washing and each of the fractions could betreated separately.

[Insert Recommedations on Stabilization/Solidification Here]

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fiR302599

SECTION 3

EXPERIMENTAL DESIGN AND PROCEDURES

3.1 SAMPLE"ACQUISITION AND CHARACTERIZATION

Personnel from EPA Regions II, III, IV, VI, and X provided PEI withrepresentative 5-gallon samples of soil and battery casings from each sitefor use in the soil washing and solidification/stabilization (S/S) studies.Sampling personnel at each site collected the samples from locations thoughtto have the highest concentration of contaminants. The samples were .collected via both grab and composite sampling procedures. However, allsamples were homogenized to the practical extent possible to attempt toprovide a uniformly contained sample. The samples were then placed in new,plastic, 5-gallon pails and were sealed with plastic lids, taped, and labeledfor shipment as environmental samples. All treatability testing wasconducted at the laboratory facility of the Illinois Institute of TechnologyResearch Institute (IITPI) in Chicago, under their RCRA RD&D permit. BothPEI and IITRI personnel participated in the testing program.

Upon receipt of the samples at IITRI, pieces of the battery casinglarger than 3/8 inch were ground into smaller sizes to release Pb particlesand to liberate any adhering residue. As a means of minimizing the vari-ability in duplicate test results and increasing the homogeneity of thematerial, each soil/debris sample was mixed thoroughly in a "V" type blenderfor 10 minutes.

Samples of the raw soil from each of the six sites were characterizedfor physical and chemical properties, including grain size distribution,moisture content, pH» cation exchange capacity (CEC), humic acid, totalorganic carbon (TOC), and lead (total and Teachable). The predominant soilminerals and lead species, as indicated by X-ray diffraction, were alsodetermined. The purpose of these analyses was to characterize the physicaland chemical nature of the samples before the final test was designed. Thelist of characterization analytes is summarized in Table 3-1.

The list of analytes in Table 3-1 was determined through conversationsand meetings with several experts and interested parties within EPA. Thesoil characterization analytical list, while not exhaustive, is quite exten-sive and was put together to determine whether certain characteristics of thesoil or waste material would make it more or less amenable to soil washing.To further explain the reasons each of these parameters was included in thesoil characterization, Table 3-1 lists the possible significance of eachparameter to the soil washing study.

3-1

SR3Q26QO

TABLE-3-1. LIST OF SOILS-CHARACTERIZATIONANALYTICAL PARAMETERS

Parameter . Possible significance in soil washing or S/S studies

Grain stze^v : — : Affects __dewa_tering characteristics of soildistribution :

Clay content Affects desorption characteristics of soil

Moisture content Indicates dewatering characteristics of soil

pH, S.U. . Affects "select! on of wash solution

Cation exchange Affects desorption characteristics of soilcapacity

Humic acid Possible interference in cement-based stabilization

Total organic Affects desorption characteristics of soilcarbon

Lead (total) Indicator parameter for evaluating effectivenessof wash solution

Lead (Teachable) Parameter on which performance goals are based

Predominant lead Affects selection of wash solutionspecies

Predominant mineral Affects selection of wash solutionspecies ,~:~ ;™:v . . v; :-^ .__..,.._ \ -— ..-•- -

3-2

3.2 TEST PLAN

The goal of this study was to evaluate the potential effectiveness ofsoil washing volume-reduction techniques for treating lead-contaminated soil{at the Pesses Site, removal of cadmium, copper, nickel, and lead was evalu-ated) and debris from Superfund sites. The soil washing procedures followedduring this testing and evaluation program were based on a set of four assumptions that underlie the volume-reduction approach to washing contaminatedsoils. These assumptions are as follows:

0 A significant fraction of the contaminants in soil are eitherphysically or chemically bound to the silt- and clay-sized parti-cles of the soil.

0 The silt and clay are attached to the sand and gravel by physicalprocesses such as compaction or adhesion.

0 Physical washing (e.g., scrubbing) of the sand and gravel fractionswill effectively remove the fine silt and clay materials.

0 The contaminants will be removed to the same extent that silt andclay are separated from the sand and gravel. Increasing the effi-ciency of the washing process will directly increase the removalrate.

This study involved a series of bench-scale experiments in which variousconcentrations of a chelate solution (ethylenediaminetetraacetic acid, EDTA),a surfactant solution (an anionic phosphated formulation of Tide)s and awater wash were evaluated. For the ILCO and Pesses sites, however, the soilsamples were tested by using only chelate solutions and water washes. Nosurfactant solution was used for washing the soil samples from these sites(largely because of time and budgetary constraints). The contaminated soil(particles <2 mm in diameter) resulting from washing the Gould site soil wasalso subjected to stabilization/solidification (S/S) to determine thefeasibility of adding S/S to the tail end of soil washing in a treatmenttrain approach. The S/S processes involve mixing the contaminated soil witha binding agent (portland cement) to enhance the properties of the waste byphysical and/or chemical binding of the lead in the final product. Figure3-1 presents the overall test plan used during this study.

3.3 EXPERIMENTAL PROCEDURES

3-3.1 Soil washing

A 10:1 ratio of wash solution to soil was used (i.e., 5000 ml washwater to 500 g soil) for all the tests. Reaction time was set at 30 minutes,and all tests were executed at room temperature. Each test was conducted induplicate, and each of the duplicates consisted of two 500-g soil samplestreated simultaneously. Like size fractions produced by screening/sieving ofthe two samples were combined to generate sufficient quantities of materialin all size fractions for subsequent chemical analysis.

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Figure 3-2 is a schematic diagram of the soil washing test procedures.For each 500-g sample, the soil was mixed with 5000 ml of the wash solutionin a sealed 10-liter (2.5-gallon) glass jar and agitated on a reciprocatingshaker for 30 minutes. After the contact period, the soil/water mixture waspoured over a nest of sieves (No. 10 and No. 60) and a pan to separate thewash water from larger soil fractions and to segregate the soil into three . .size fractions. Th~e sieve stack was then placed on a sieve shaker withrotational and tapping movements for 10 minutes to aid further removal ofcontaminants and as much water as possible. Next, each soil fraction wasrinsed twice with tap water (1000 ml per rinse) and placed on the sieveshaker again for 10 minutes after each rinse. The soil was then separatedfrom the wash water by wet-sieving and filtering. This operation simul-taneously segregated the soil into the following three size fractions:

Sieve size Soil fraction Particle type

1) No. 10 screen > 2-rnn fraction Gravel

2) No. 60 screen 0.25- to 2-mn fraction Sand

3) Pressure filter < 0.25-mm fraction Silt and clay(0.45 ym)

The soil fractions were then transferred to appropriate sample con-tainers and subsequently submitted to the PEI lab for analysis of lead resi-duals. Portions of the wash and rinse waters from each test were also fil-tered and analyzed for lead. For the Pesses site, the samples collected fromsoil washing experiments were further analyzed for cadmium, copper, andnickel.

In this study, three wash solutions were evaluated under ambient tem-peratures: tap water (control), a chelate solution (3:1 molar ratio for EDTAto total chelatable metals), and a surfactant solution (0.5 percent byweight). The pH values were adjusted to between 7 and 8 for the EDTA solu-tion, but were not adjusted for water or surfactant solutions. The Pessesand J&L soils were washed with water and three concentrations of EDTA solu-tions, one of which was used at two pH values. The solution concentrationswere determined on the basis of the initial sample characterization resultsand were tested in duplicate on each of the six soil samples.

The washing treatment scheme for battery casings (presented in Figure3-3) is smllar to that for soils with the exception that the casings werefirst shredded to less than 3/8 in. to release any interstitial lead par-ticles and to liberate any adhering residue. The casings then were washed,and the rubber particles and sludge were separated by wet-sieving, rinsedwith water, and analyzed for total lead. As in the soil washing experiments,tap water (control), a chelate solution, and a surfactant solution at ambienttemperatures were tested in duplicate on the battery casing sample. (Ap-pendix A outlines the detailed experimental procedures for the soil washingevaluations.)

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3.3.2 Solidification/Stabilization of Residual Fines

For the Gould site only, samples of the residual soil fractions from thethree washing solutions (water; chelate, and surfactant) were mixed individ-ually with a solidification agent (port!and cement) to evaluate the effect ofa cement-based S/S process on the immobilization of the lead in the soilfraction "consisting of particles <2 mm in diameter. The material was mixedat a cement-to-soil ratio of 0.25 and a water-to-total-solids ratio of 0.4.After a 14-day curing period, the solidified product (crushed and monolithic)plus an unsolidified'sample were subjected to the monofilled waste extractionprocedure (MWEP) (SW-924, 2nd Edition, January 1986), and the extracts (fourper sample) were measured for pH and analyzed for total lead. Figure 3-4 isa schematic diagram fo"r solidification/stabilization of the fines from theGould site. (Appendix A details the experimental procedures for the stabi-lization evaluations.)

3.4 SAMPLING AND ANALYSIS ;

Sampling and analysis procedures specified in the general soil washingQuality Assurance Project Plan (QAPjP) prepared under this contract {Task19B) and the project-specific QAPjP developed for this set of experiments(Tasks 19G, 19H, and 190) were followed in the performance of this work. Thecomposite sample obtained from EPA regional personnel from each site wasthoroughly mixed in a V-blender for 10 minutes. Aliquots were then collectedfor characterization analysis and the treatability tests.

Total lead (for Pesses site—total cadmium, copper, lead, and nickel)was measured by EPA method 6010 (ICAP). EPA Method 3050, acid digestion, wasused for sample preparation. This preparation method uses concentratednitric acid and hydrogen peroxide to solubilize all lead (and other metal)compounds. Lead chloride is the only lead compound that may not besolubilized by EPA Method 3050. Lead chloride, however, was not present inthe soils tested. Accuracy goals were set at 75 to 125 percent for totallead in water and 75 to 125 percent for total lead in soil. Precision goalsfor all matrices were set at ±20 relative percent difference. Completenessgoals for all analysis were set at 90 percent.

The following procedures were used to obtain TCLP and EP Toxicityresults:

. ° TCLP: 51 FR21648, June 13, 1986.

EP Toxicity: Method 1310, SW-846, 3rd Edition, 1986.

The extracts produced by these procedures were analyzed for lead by EPAMethod 6010. Because of the concentrations of cadmium, copper, and nickelresiduals in the soil from the Pesses site, however, extracts were analyzedfor these metals in addition to lead. The accuracy, precision, and complete-ness goals for the TCLP and EP Toxicity extracts were the same as those citedherein for total metals measurements.

3-8

R302607

WaterWash

SurfactantWash

ChelateWash

UNSOIIDIRED SOLIDIFIED

PARTICLE SIZE DISTRIBUTIONMOISTURE CONTENT

HUMIC ACIDpH (solid)

TOTAL LEAD (extract)TCLP

pH (extract)

Number of Samples:

TCLP

pH (extract)

Particle Size Distribution = 3x2 =6Moisture Content« 3x2x2 =12

Hurnic Acid Content = 3x2 =6pH (solid) = 3x2 =6

Total Lead (solid) » 3x2 =6TCLP = 2x3x2 =12

Total Lead (extract) - 3x2x2 =12pH (extract)- 2x3x2 =12

Figure 3-4. Solidification and stabilization studies.

3-9aR3Q26QrJ

TABLE 3-2. ANALYTICAL MATRIX

No. of Analyses

Sample - Total Pb E.P TOX Pb TCLP . Other

Characterization Studies

Raw soil •— 22 ... 16 4 16 HSL, CN, F, S,humic acid, XRD,CEC, TOC, grain,moist, pH

Casings battery 3 3 2 HSL, CN, F, S,humic acid, XRD,CEC, casings, TOC,grain, moist, pH

Washing studies _ ._.:,„ .__ _ „____. :- -

Battery casings

Rubber 6 2Sludge .. 6 __ _ _2____Wash solution 6

Soils

Soil >2 mm 47 24 12 10 total Cd, Cu, Ni;6 TCLP Cd, Cu, Ni;6 EP tox Cd, Cu, Ni

Soil 0.25 to 2 mm 47 24 12 10 total Cd, Cu, Ni;6 TCLP Cd, Cu, Ni;6 EP tox Cd, Cu, Ni

Soil <0.25 mm 47 24 -12 1C total Cd, Cu, Ni ;6 TCLP Cd, Cu, Ni;6 EP tox Cd, Cu, Ni

Wash solution 47 10 total Cd, Cu, Ni;6 TCLP Cd, Cu, Ni;6 EP tox Cd, Cu, Ni

Rinsate No. 1 23 106 TCLP Cd, Cu, Ni;6 EP tox Cd, Cu, Ni

(continued)

3-10

TABLE 3-2 (continued)

No. of Analyses

Sample Total Pb EP TOX Pb TCLP Other

Riru, ."o. 2 23 10 total Cd, Cu, Ni;6 TCLP Cd, Cu, Ni;6 EP tox Cd, Cu, Ni

Stabilization studies

Unsolidified solids 6 66 humic acid,grain, pH;12 moist

Solidified solids 6

Qualit" assurance .

Soi. 2 MS/MSD 1 MS/MSD 1 MS/MSDSoil c.. 2 mm 3 MS/MSDSoil <0.> 12 MS/MSD 1 MS/MSD 1 MS/MSDWash/rinse: 13 MS/MSDUnsolidifiea solidsSolidified solids

3-11

flR302610

The analytical matrix presented in Table 3-2 shows the type and numberof samples that were analyzed after each test, the analyses that wereperformed on the untreated soil, and the QA/QC samples (matrix spike/matrixspike duplicates) that were analyzed.

3-12

SR3026

SECTION 4

BUREAU OF MINES APPROACH

The Bureau of Mines (BOM) has been actively involved in the treatment ofsoil and battery casings with washing and leaching processes. The Bureaucurrently has an Interagency Agreement (IA6) with EPA at the C&R, Gould, andthree other Superfund sites to assess the applicability of a cleanup techno-logy for battery casings that the Bureau is developing and to assist the EPAProject Officers on related technical issues. The Bureau is currently work-ing on fine-tuning a process based on fluosilicic acid leaching and electro-winning that will be ready for field trial in mid to late 1990. The Bureauhas conducted laboratory work in support of the development of this process;the laboratory efforts are constantly being adjusted to identify the mostcost-effective and technically feasible approach possible.

In 1987, the Bureau began investigating the use of EDTA in these pro-cesses at the United Scrap Lead (USL) site in Ohio. The Bureau researchersconcluded that EDTA is an excellent solubilizer, but that its use in thefield presents some problems. These include:

0 Filtering difficulty0 Recycling problems0 Greater cost and complexity0 Problems with recovery of Tead from the EDTA solution.

The Bureau is also investigating processes based on the use of fluosi-licic acid to leach lead from soils and battery casings. In these processes,the lead sulfate and lead dioxide are converted to lead carbonate, which issoluble In fluosilicic acid. After the lead is leached with fluosilicicacid, it is subjected to electrowinning to remove it and the acid is recycledback to the leaching process. Further leaching with nitric acid may increaselead removal.

The Bureau has looked at the EDTA and fluosilicic acid washing andleaching processes on a site-by-site basis at several Superfund sites, mostlyin Region V. Because the Bureau is constantly adjusting its laboratoryefforts to identify the most cost-effective solution for remediating leadbattery Superfund sites, standard operating procedures are not readily avail-able for their work. At the request of the U.S. Environmental ProtectionAgency, PEI has investigated the use of EDTA on six soils and a standard soilmatrix (SSM), the use of surfactants on four of these soils, and the use ofeach of these solutions on battery casings from the Gould site. PEI's role

4-1

/5R3Q2612

was to investigate the efficacy of the use of EDTA, surfactants, and fluosi-licic acid in relation to site characteristics, including grain size distri-bution, mineralogy, and lead speciation. The intent of this effort was todevelop a small data base covering the technical feasibility of using each ofthese wash (or leach) solutions"to remediate sites with particularcharacteristics. Because the testing was conducted concurrently on many ofthe sites by the same researchers who were following standard operatingprocedures, the resulting data are directly comparable between soils fromdifferent sites, between different washing solutions, and between soils andbattery casings. PEI developed a laboratory test procedure based onavailable knowledge of the Bureau approach; however, lack of funds preventedconducting tests using the Bureau approach. In conducting these tests, PEI'sgoal would be to gather data on the use of fluosilicic acid on soils fromseveral Superfund sites directly comparable to those involved in tests on theuse of EDTA and surfactants.-

The statement of work for PEI has assumed that these experiments fallinto the category of screening studies rather than process optimization. Inscreening studies, the goal is solely" to show Whether the technology beinginvestigated is technically feasible for meeting the performance goals of thesite (i.e., in terms of total and leachable lead in the residual soil). Thegoal of process optimization, however, includes developing data to scale upto pilot- and full-scale tests and to estimate costs. Both of these activi-ties require exploring the entire process scheme, including the treatment orrecycling of wastewaters and the recovery of lead from these wastewaters.

The most contaminated fraction of soil is expected to be the fine par-ticles, which may require additional or more aggressive treatment comparedwith that required for the larger soil fractions. PEI has collected data onthe use of solidification/stabilization to reduce the mobility of the leadremaining in the residue. The Bureau's work to date has assumed that leadwill be leached by use of fluosilicic and/or nitric acids, that the lead willbe recovered electrolytically, and that the acid will be recycled. TheBureau is also investigating the possibility of selling,the lead-contaminatedsludge to a smelter, which would entail significantly less capital cost andcomplexity than an additional leaching step.

4.1 BUREAU OF MINES LEACH-ELECTROLYTIC TECHNOLOGY

Early studies at the Bureau's Avondale Research Center in Avondale,Maryland, involved developing an electrolytic process to recover lead fromscrap batteries (see "Economic Evaluation of an Electrolytic Process toRecover Lead From Scrap Batteries," 1985, by Thomas A. Phillips). Figure 4-1is a schematic of the process. In this process, scrap batteries are crushedand separated into metal and sludge fractions. The metal fraction is castinto anodes and electrorefined. Lead in the sludge fraction is converted tolead carbonate by reaction with an ammonium carbonate/ammonium bisulfitesolution. The lead carbonate is then dissolved in a fluosilicic acid electro-lyte from which the pure lead metal is separated by electrowinning. An

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alternate leaching process suggested in this report involved Teaching leadsulfate, but not lead dioxide, out of the sludge. This modification wouldeliminate the need for ammonium bisulfite and result in a simpler process.The leach residue, consisting of lead dioxide, could then be sold to a smelter,

Rubber Battery Casings

After the work on recovering lead from scrap batteries was completed,the Bureau began testing the leach-electrolytic technology on battery casingsfrom the United Scrap Lead (USL) site. The tests were conducted on 2-kgsamples consisting of 70 percent rubber, 15 percent sludge, 3 percent metal-lic lead, and 12 percent moisture. The process under investigation involvedfive steps: 1) washing/leaching, 2) screening and filtering, 3) furthercleaning of the casing material, 4) leaching of the sludge residue, and 5)electrowinning. r ""'" ~' " " ~ ----^- ,-, - - ._..

For the washing/leaching step, 2 kg of battery casing material wasleached with 3.5 liters for 1 hour in a ball mill. Table 4-1 presents thesummary data collected.

TABLE 4-1, BUREAU OF MINES DATA FOR WASHING BATTERY CASINGS

Residual rubberWash Solution casings, ppm Pb Comments

(NH4) acetate (4%) + 2250 Readily filterableacetic acid (3.5%)

Tetra-Na EDTA (5%) or 1563 Extremely difficult toDi-Na EDTA (5%) filter

Tap water 2500 Readily filterable

Surfactant Not yet available

The material remaining after the wash step was wet-screened with 3/8-,8-, and 16-mesh screens, and the water and sludge were filtered through No. 2Whatman filter paper. The sludge contained 23 to 36 percent lead, dependingon the wash solution used. The filtrate could potentially be used in thesludge leaching step. The researchers noted that metallic lead would probab-ly be removed in the field by gravity separation.

After the screening and filtering step, the casing material was treatedby several methods, including sonic cleaning, for further reduction of thelead content. A 5 percent EDTA solution produced the most promising results.Table 4-2 presents a summary of the results.

4-4

flR3026!5

TABLE 4-2. RESULTS OF CLEANING BATTERY CASINGS IN 5 PERCENT EDTA SOLUTION

Method Pb remaining, EP Tox test,ppm ppm Pb

1-day soak, 15-minutesof sonic cleaning 540 443-day soak, 30-minutesof sonic cleaning 370 Not determined6-day soak 76 15.5 -

In another test, the casings were soaked for 3 days in a 5 percent EDTAsolution, followed by a 15-minute sonic cleaning in distilled water to whicha wetting agent had been added. The lead content of the resulting casingswas 30 ppm, and the EP Toxicity result was 5 ppm. These promising resultsled to subsequent investigations with additional wash solutions.

The fourth step of this process was to leach the sludge remaining fromthe screening and filtering step. Table 4-3 presents the results.

TABLE 4-3. RESULTS OF SLUDGE LEACHING TESTS

Temperature Pb Extraction, Pb inLeach solution °C Time, h % residue,%

Tetra-Na EDTA 55° 2 85 15

Tetra-Na EDTA + 55°temp 2DI-Ha EDTA 1 99 1

(NHJ?C03 * NHAHSO- 55° 1+ HjjSIFg * J 50 1 97 3

(NH-) acetate + 70 2 34.3 NotaSetlc acid determined

The relatively poor results achieved with the tetra-Na EDTA suggest thatdifferent lead compounds are selectively chelated. Therefore, the research-ers conducted solubility testing with different lead species and differentforms of EDTA. These results are presented in Table 4-4. As shown, disodiumEDTA removed all of the lead dioxide but none of the lead sulfate; whereastetra-sodium EDTA had the opposite results. These data indicate that an EDTAwash process at a site with a combination of lead sulfate and lead dioxidemay require multiple treatment stages with different forms of EDTA.

4-5

TABLE 4-4. SOLUBILITY OF LEAD COMPOUNDS IN EDTA

Percent removed

EDTA

Di-NaTetra-Na

PH

510

Pb02

1000.0

PbS04

0.0100

Pb metal

2.723.6

The last step involved electrowinning the lead from the fluosilicic acidsolution. The use of"a'nonmembrane cell with lead-dioxide-coated titaniumanodes and both stainless steel and lead cathodes achieved lead concentrationsof less than 1 ppm in the resulting solution. Recovering lead from ammoniumacetate solutions was also successful.

Based on this work, researchers prepared an economic assessment of ahypothetical process to treat battery breaker residue (see "InitialAssessment of the Economic Potential of a Hypothetical Process to TreatBattery Breaker Residue using Leach-Electrowinning Technology," by Thomas A.Phillips, September 1987, Bureau of Mines Internal Report). Because of thepractical difficulties with the EDTA solutions, the assessment was performedwith a fluosilicic acid leach process. Figure 4-2 is a schematic of thisprocess. The process calls for a retention time of 1 hour and a temperatureof 55°C for the ammoniacal leaching step, a retention time of 8 hours and atemperature of 50°C for the rubber leaching step, and a retention time of 1hour and a temperature of 50°C for the sludge leaching step. The estimatedtotal capital cost is $7.6 million, and the net operating cost is $150 perton of waste rubber processed.

Leaching Lead from Soils

Bureau of Mines researchers also conducted some tests on soil samplesfrom the USL site that contained 8400 ppm lead (0,84 percent). Table 4-5presents a summary of the results. The EDTA achieved a high removal efficien-cy, but it was extremely difficult to filter; filtering and washing the soilresidue required 3 days. The best results were achieved by using carbonationand a fluosilicic leach followed by a dilute nitric acid leach for 72 hours.This process resulted in a leachate residue containing 400 ppm lead, with EPToxicity results of the soil less than 1 ppm. The Bureau prepared a reportentitled "Conceptual Process Design and Cost Estimate for Removing Lead FromSoil at the United Scrap Lead Superfund Site." The conceptual process isshown in Figure 4-3. The carbonation and acid leaching portions of theprocess require retention times of 1 hour and temperatures of 55°C. Theestimated cost of the hypothetical soil treatment train was $205 per cubicyard, which is in the range of the $200 per cubic yard for landfill disposal.

4-6

fiR302617

Battery breaker resifiua

1GRIZZLY Overs lie

MAGNETIC SEPARATOR

1Tramp Iron

SHREDDER

AtttOKIACAL LEACH

ISCREEN

LEACH SOLUTIOHRECOVERY

1RUBBER LEACH

FILTER

Clean sludge — FILTER

FILTER

SLUDGE LEACH/

I

rubber

ELECTROVIHNING

Lead

Figure 4-2. Bureau of Mines conceptual process for treating batterybreaker residue.

4-7

SR3026I8

TABLE 4-5. SUMMARY OF PRELIMINARY RESULTS FROM SOIL WASHING OFUNITED SCRAP LEAD SOIL

Pb Pbextraction, in leachate,

Leaching method % ppm

3-Day water leach 0.06 0.67

3-Day dilute aceticacid leach0.025 N 20g— 100ml 0.075 1.20.05 N 20g--100ml 0.682 10.40.10 N 20g— 100ml 3.67 58.3

1-Day 4% HN03 leach _ _ _ . . _30.0 ._ .1000

EDTA leachEDTA at pH_ll, and - 99+ 2830adjusted to pH~5 . . . . . .with acetic acid

Two-step leaching1) Carbonation (1 h)2) H2SiF6 leach (1 h) 33.8 1900

Three-step leaching1) Carbonation (1 h)2) 4% HNO. leach (24 h)3) H20 soik (72 h) 63.7 1600

Three-step leaching1) Carbonation (1 h)2) H.SiF, leach

(1 h, acid recycled) 72 1912Followed by:3) Leaching with a

1/2% HNO-/H«0 sol'nfor 72 hfs/ -100 - 185

Pbin soil residue,

ppm

8100(estimated by diff.)

810081008100

(estimated by diff.)

6800(estimated by diff. )

140(by analysis)

5380(estimated by diff.)

3050(estimated by diff.)

2710(estimated by diff.)

400(estimated by diff.)

a This process required 3 days to filter and wash soil residue.Easy to filter and wash.

4-8

SR3026I9

Soil

Water

To waste water treatment

To waste water treatment

Lead-free toil

Figure 4-3. Bureau of Mines conceptual process for treatinglead-contaminated soil.

4-9

3R302620

4.2 COMPARISON OF BUREAU OF MINES AND PEI TREAtABILItY STUDIES

Numerous differences exist between the test methods used by the Bureauof Mines and PEI for soil and battery casing washing with EDTA. Each useddifferent solid-to-liquid ratios, pHs, retention times, and agitation meth-ods. Also, the starting lead concentration at the United Scrap Lead site wasgenerally lower than that of most of the sites investigated by PEI. TheBureau work does show that given enough time and agitation, most of the leadcan be removed from the soil; however, several practical problems need to besolved before field implementation is attempted.

Based on the available information on the Bureau's approach to the useof fluosilicic acid, PEI prepared a laboratory test plan designed to simulatethe Bureau's work and to develop data comparable to that collected with theuse of EDTA and surfactant solutions. Budget constraints and lack of furtherdetails concerning the Bureau laboratory work, however, prevented tests frombeing conducted. The standard operating procedures for the proposed PEIlaboratory studies using soil and battery casings are given in Appendix A.

4-10

8R30262I

SECTION 5

RESULTS AND DISCUSSION

5.1 SAMPLE CHARACTERIZATION

Results of the sample characterization are presented in Table 5-1. Thedata shown represent averages of two or more data points. Appendix B con-tains a more complete presentation of the data. The data presented werecollected from soil washing experiments conducted at two different times--first on the J&L Fabricating and Pesses soils and subsequently on the otherfour soils and the Gould battery casings.

Particle size, mineralogy ...___!_.

Soils from the Schuylkill, Gould, and J&L Fabricating sites contain arelatively large percentage of sand and gravel, whereas soils from the OldMan's Township, C&R, and Pesses sites contain a relatively high percentage ofsilt and clay. The_ predominant mineral species for most sites are quartz andcalcite (CaCCL), except for the Gould site, where the predominant species arequartz and Nai Ca-feldspar. The calcium content of the soils generallyconfirms the finding of calcite mineralogy; however, the Gould soil containsmore calcium than does the Old Man's Township soil. The calcite peak for theOld Man's Township soil was very small, which is confirmed by the low calciumconcentration (1020 ppm). In summary, the C&R, Schuylkill, O&L Fabricating,and Pesses sites contain carbonate soils, the Old Man's Township site con-tains a slightly carbonate soil, and the Gould site contains a non- carbonatesoil.

Lead Speciation

Table 5-1 also indicates the predominant lead species for each of the _sites, which are as follows: Old Man's Township and Schuylkill, lead car-bonate (PbCOJ; C&R, hydrocerussite [Pb-(CO-)«(OH)?]; Gould, lead sulfate(PbSO,) and Tead dioxide (Pb02); and O&t Fabricating, lead hillite[Pb-SO-tCQ-WOH^]. The lean species at the sites with carbonate soils isgenerally a carbonacious form of lead, such as lead carbonate, hydrocerus-site, or lead hillite. The only noncarbonate soil was from the Gould site(the only site with Na, Ca-feldspar instead of calcite), where the pre-dominant lead species are lead sulfate and lead dioxide. Lead sulfate andlead dioxide are also the primary lead forms in a lead-acid battery in ad-dition to metallic lead. Therefore, the lead carbonate may result from achemical reaction between the lead forms that are deposited on the site andthe carbonate that is present in the soil.

5-1

R302622

TABLE 5-1« SAMPLE CHARACTERIZATION

Parameter

Grain tlze distributionSand and gravel, wt "iSilt, wt. IClay wt, I

Predominant mineral2spectes

Predominant clayspecies

Moisture content, 5C

pH, S.U.

Cation exchange capacity,meq/100 g

humic acid, 1Total organic carbon,us/kg

Lead (total), mg/fcg*1Lead (total), mgAgf

Average total le»d. Kg/kg

EP toxicity, ms/liter*1'1

TaP lead, ma/liter5Predominant leadspecies

Aluminum

Calcius

Iron

Old Kan'sTownship

691714

Quartzcalcite(minor)

Illitekaolinite

7.2

6.18

36.5

0.34

16,000

57.150

19,700

h 48,000

300

984

PbOLj

1,665

1,020

22,850

C&R

553114

Quartzcalcite

Illitesmectite

17.5

9.34

36.6

0.04

7,015

75,850

53,400

68,4000

413

330

EVCQ-V?OH}|2

4,700

57,900

5,795

Schuylkill

8767

Quartzcalcite

Smectite

5.5

7.24

40.2

0.76

14,150

3,230

7,640

4,700

55.5 .

85.5

PbC03

3,025

- " 43,400

3,230

Gouldsoil

9154

QuartzHa, Ca-feldspar

Smectl teIllite

. 2.4

6.50

23.5

1.21

5,555

27,150

28,400

27,600

- 148

657

. PbSO /Pb°2

. 9,930

. 6,910

..22,150

J&LFabricating

9082

QuartzcalcitedolomiteKaolinitesmectite

8.8

6.31

5.2

NAC

3,588

3,945

5,194

4,194

196

NA

Pb.SO.-(co372(OH)218,475

72,700"

15,475

Pesses

632017

Quartzcalcite

KaoliniteIllitesmectite

10.7

6.55

13.4

HA

14 ,500

302e

210s

271

0.171

0.297

NA

4,540

65,600

23,750

Gouldbatterycasings

52444

Quartz

IlUtesmectite

3.0

5.44

21,2

0.13

50,300

263,500

101,000

209,000

1830

1360

PbSO./Pb°2970.5

3,670

20,500

? Dolomite • (Ca.HgJCQ,; Calcite • CaCQ,; *nd Quartz » 510,.* Kaolinite • AVtJL*(OH)4; Smectite * Na-Ca-Al-Si-O-H; 3nd Illlte - K-Al-Si-Q-H. . ,5 HA • not analyzed 3^ Initial characterization, average values.! Pesses Is a nickel-cadmium site. Average concentrations: cadmium « 1,500 yg/g; nickel - 1,520 ug/g; copper « 4,255,Characterization during testing.

? Concentrations: cadmium * 1.948 ng/g, nickel • 2,131 ug/g; copper « 1,680 pg/g." Average of all concentrations given In Appendix C.; EP Toxicity for cadmium * 23,0 »s/L; for copper - 2.51 mg/L; for nickel » 3.gi mg/L.•* TaP for cadmium - 24.4 mg/t; for copper • 5.00 ag/L; for nickel • 5.83 m)/L.

5-2

flR302623

Other characterization parameters .

The moisture content of all the soils studied ranged from 2.4 to 17.5percent; the soils at the Gould site had the lowest moisture content (andlowest silt/clay content), and soils at the C&R site had the highest moisturecontent (and highest silt/clay content). Soil pH is around neutral for allthe soils except those at C&R, which are slightly alkaline. The pH for theGould battery casings is slightly acidic (5.44), possibly as a result ofsulfuric acid contamination from the electrolyte used' in the batteries. Thecation exchange capacity for all soils is less than 40 meq/100 g. The humicacid content of the soils is lowest at the C&R site (0.04 percent) and highestat the Gould site (1.21 percent). Soils from the C&R, Gould, and J&LFabricating sites have a low total organic carbon (TOC) content, and soilsfrom the Old Man's Township, Schuylkill, and Pesses sites have a high TOCcontent. The Gould battery casings have a high TOC content (50,300 mg/kg)because the rubber casings are organic.

Total and teachable Lead = ___

Total lead concentrations for all soils and battery casings in Table 5-1are provided for two samples: those resulting from the original samplecharacterization and samples taken during testing. The sample from thePesses site shows a low lead concentration (210 to 302 mg/kg) because thesjte processed nickel-cadmium rather than lead batteries. Samples from theSchuylkill and J&L Fabricating sites show the next lowest lead concentrations(approximately 3000 to 8000 mg/kg), and those from the Old Man's Township,C&R, and Gould sites show the highest contamination (27,000 to 76,000). Forsome samples, the two values vary widely, which is indicative of the vari-ability of the soils and the resulting difficulty of collecting a representa-tive sample for analysis. Particles of lead present in an analytical samplecould result in a nonrepresentative analysis. The Gould battery casings havethe highest lead concentrations (101,000 to 263,500 mg/kg) and the highestvariability, probably due to the presence of large chunks of casings.

Table 5-1 also presents data on leachable lead. The EP Toxicity resultswere collected from the initial characterization samples, whereas the TCLPresults were obtained from the samples that were collected duringactual testing. The J&L Fabricating soils were subjected only to the EPToxicity test. All EP Toxicity test results are above the regulatory limitof 5.0 mg/L for defining a hazardous waste (except for Pesses, which is anickel-cadmium battery site); the lowest result (for soils from the leadbattery sites) is 55.5 mg/L for soils from the Schuylkill site; the highestresult is 418 mg/L for soils from the C&R site (these correspond to thelowest and highest soil concentrations). The EP Toxicity result for theGould battery casings was 1830 mg/L. The Pesses soil is hazardous because ofthe amount of leachable cadmium it contains (23.0 and 24.4 mg/L in the EPtoxicity and TCLP extracts, respectively); the regulatory limit is 1.0 mg/L.

5-3

5.2 SOIL WASHING TESTS

Appendix C presents extensive summaries of the raw data. Results pre-sented in this section are discussed in terms of average values of replicatetest runs and analyses.

Numerous types of data were collected during this study, includingweights of all soil fractions, lead concentrations in each soil fraction andwash solution, and TCLP results for many of the soil fractions. Results arepresented in terms of soil collected on different sieve sizes. The followinglist presents the size of the particles collected:

0 No. 10 sieve—particles > 2mm

0 No. 60 sieve—particles from 0.25 to 2mm

0 Pan—particles that settled in the bottom pan under the No. 10 andNo. 60 sieves, < 0.25 mm

0 Filter—particles that were carried into the wash or rinse solutionsand were collected by using a pressure filter.

0 Fines—combination of the pan and filter particles.

Size Distribution

Table 5-2 presents the weight percent of soil collected in each soilfraction (< 0.25 mm, 0.25 to 2 mm, and > 2 mm). The percentages given inTable 5-2 represent the minimum amount of potential weight reduction thatcould be achieved if only some soil fractions could be cleaned enough to meetthe performance standards for a particular site. For example, cleaning theGould No. 10 and No. 60 fractions well enough to be backfilled on site wouldresult in at least an 83 percent reduction in the amount of lead-contaminatedsoil that must be further treated or disposed of offsite. For some sites(e.g., Old Man's Township), the fraction of No. 10 soil is not high enough tojustify a soil washing process if this is the only fraction that could besufficiently treated.

Lead Concentrations in Soil Fractions

Table 5-3 presents average values of lead concentrations in each of thethree wash solutions and three soil fractions collected from the Old Man'sTownship, C&R, Schuylkill, O&L Fabricating, and Gould soils and the Gouldbattery casings. Figures 5-1 through 5-6 depict graphical representations ofsoil fraction concentrations compared with the untreated soil lead concentra-tions. Table 5-4 presents the lead, nickel, cadmium, and copper results forthe Pesses soil, and Figures 5-7 through 5-10 depict the graphical representa-tions. The relative heights of the bars in Figures 5-1 through 5-10 indicatethe relative concentration of metals in each of the soil fractions. Theminimum and maximum values of the metal concentrations in the untreated soil

5-4

AR-302625

from the.initial characterization and from sampling during testing have beenincluded for baseline comparison. Both of these lead concentration valueswere included to indicate the sensitivity of the results and conclusions tothe representativeness of the analytical sample and variability of the totallead concentration in the untreated soil.

TABLE 5-2. DISTRIBUTION OF SOIL COLLECTED IN EACH FRACTION(weight percent)

Site

Old Man'sTownshipC&RSchuylkillGould soil

J&L Fabri-catingPesses

Gould casings

>2mm(No. 10)

9

281615

17

18

44

0.25-2mm(No. 60)

47

293468

" 65

__...__32

NCb

FinesPan

19

183511

„

— —

40

(<0.25mm)aFilter

25

25156

— —

17

Totalfines

44

435017

19

50

57

-Fines * Pan and filterDNC = Not collected

Table 5-5 presents the percent removal of lead advieved for each of thesoil fractions. These data have been calculated from the analytical datapresented in Table 5-3, and represent quantitative information for the graphsshown in Figures 5-1 through 5-6. Table 5-6 presents the percent removal ofcadmium, copper, lead, arid nickel from the Pesses soil. The metal concentra-tions used in these calculations were average values from all data points inAppendix C. Negative numbers indicate an increase in metal concentrationcompared with the untreated soil.

The cited benefits of soil washing include the theory that much of thelead and other contamination is concentrated in the finer fractions; andtherefore, the larger fractions should have lower lead concentrations afterwashing than the soil as a whole had prior to washing. The surfactant anachelate washes would also be expected to improve the removal of lead fromeach of the soil fractions; thus, these fractions should contain lower con-centrations than the soil washed with water. In general, therefore, thegraph bars for the fine fractions in Figures 5-1 through 5-10 should betaller than those for the larger fractions, and the bars for the water wash

5-5

R302626

TABLE 5-3. Pb CONCENTRATIONS IN SOIL FRACTIONS AND FILTRATES(results in ppm)

Site

Old Man's Township

CSR

Schuylkill

Gould Soil

Gould Casing

. -Wash solution

WaterSurfactantEDTA

WaterSurfactantEDTA

WaterSurfactantEDTA

WaterSurfactantEDTA

WaterSurfactantEDTA

WashSolution filtrate

J&L Fabri- Watereating EDTA,

EDTA,EDTA,EDTA,

, 0.430.0084 M* 3210.0126 M 3800.0168 M£ 4560.0168 M° 416

Wash

Soil fractions

>2 mm 0.25-2 mm <0.25 mmfiltrate #10 #60 Fine

0.79154

1,255

0.2416.5942

0.3238.473.5

0.82127324

1.32384133

Rinse1-

0.42106

67.9128

92.0

153,100 22,300 45,90098,100 32,000 36,450119,050 24,550 413250

50,150 52,200 49,50066,500 49,670 52,100164,200 57,350 24,170

893 2,160 2,9491,580 1,755 2,645886 2,340 3,995

31,350 12,800 41,40025,610 10,960 79,6508,965 8,670 15,250

35,700 - 137,65044,290 - 106,50042,500 - 116,500

Rinse2 £10 .. .#60 Fine

0.42 .6,487 2,020 13,6984.7 7,578 1,372 6,1942.8 13,236 2,717 6,6689.4 1,081 -1,516 4,6934.3 4,905 1,279 4,942

a pH = 7-8b pH - 11-12

5-6

SR3Q2627

200000

Water runsSurfactant runsEDTA runs

Untreated soil, No. 10 No. 60 FinesMin./Max. Values ~.. : .

Figure 5-1. Old Man's Township: Total Pb concentrations in washed soil fractions.

200000

Water runsSurfactant runsEDTA runs

Untreated soil, No. 10 No. 60 FinesMin./Max, Values

Figure 5-2. C&R: Total Pb concentrations in washed soil fractions.

5-7

SR3Q262S

8000

Water runsSurfactant runsEDTA runs

Untreated soil. No. 10 No. 60 FinesMinYMax. Values

Figure 5-3. Schuylkill: Total Pb concentrations in washed soil fractions.

ROQOO

Water runsSurfactant runsEDTA runs

Untreated soil. No. 10 No. 60 FinesMin./Max. Values

Figure 5-4. Gould soil: Total Pb concentrations in washed soil fractions.

AR3Q2629

300000

Water runsSurfactant runsEDTA runs

Untreated casings, No. 10 FinesMin./Max. Values

Figure 5-5. Gould casings: Total Pb concentrations in washed soil fractions.

2000060

W Water runs• EDTA, 0.0084 M^ EDTA, 0.0126 Mn EDTA, 0.0168 MM EDTA, 0.0168 M"

*pH = 11-12

Untreated soil, No. 10 No. 60 FinesMin./Max. Values

Figure 5-6. J&L Fabricating: Total Pb concentrations in washed soil fractions.

5-9

R3026

TABLE 5-4. Pb, Cd, Ni, AND Cu CONCENTRATIONS IN SOILFRACTIONS AND LIQUID FILTRATES FOR PESSES SOIL

(results in ppm)

Metal

Lead

Cadmium

Nickel

Copper

Solution"

WaterEDTA,EDTA,EDTA,EDTA,

ViaterEDTA,EDTA,EDTA,EDTA,

WaterEDTA,EDTA,EDTA,EDTA,

WaterEDTA,EDTA,EDTA,EDTA,

0.01060.01480.02100.0210

0.01060.01480.02100.0210

0,01060.01480.02100.0210

0.01060.01480.02100.0210

MaHaMMb

MaM

Mb

HaMaMKb

HaMM?K.

Wash Rins,e Rinsefiltrate 1 ... _ 2

<03454

020222628

04652

018192215

.062

.7

.7

.4

.6

.20

.9

.4

.9

.8

.44

.8

.1

.3

.7

.07

.7

.2

.2

.4

O.062 __<0.0621.51.31.91.8

0.137.75.48.47.9

0.192.32.42.51.9

0.037.75.18.26.0

0.160.380.350.38

0.081.31.81.81.5

0.190.380,800.690.59

0.021.3

_ 1.7. 1.8" 1.5

#10

41.820.220.129.525.8

501844

1191294318

2306653186525730

225139210262199

#60

312242374408300

16123618185016512635

53545736872062434966

52923916705168026123

Fines

1111.1.079.72.89.

9221041922723111

114913121882906938

9281161738668799

494

a pH = 7-8b pH = 11-12

5-10

5R302631

Water runso Jw-i • M fa = EDTA, 0.0106 M« . • § ? 1 0 EDTA, 0.0148 M| 200- J lU n EOTA,0.0210Mg . • EN 1 § EDTA,0.0210M*

0-Untreated soil, No. 10 No. 60 Fines

Min./Max. Values

Figure 5-7. Pesses: Total Pb concentrations in washed soil fractions.

Water runsEDTA, 0.0106 MEDTA, 0.0148 MEDTA, 0.0210 MEDTA, 0.0210 M*

»pH = 11-12

Untreated soil, No. 10 No. 60 FinesMin./Max. Values

Rgure 5-8. Pesses: Total Cd concentrations in washed soil fractions.

5-11

flR302632

0

10000

m Water runs• EDTA, 0.0106 M0 EDTA, 0.0148 MD EDTA, 0.0210 MM EDTA, 0.0210 M*

__ _ _ __ __ _ *pH* 11-120-Untreated soil. No. 10 No. 60 Fines

Min./Max. Values

Figure 5-9. Pesses; Total Ni concentrations in washed soil fractions.

8000" j —•

g 6000- | ^ g H Water runsEDTA, 0.0106 M

4000 4 • Ua • P EDTA, 0.0148 MEDTA, 0.0210 MEDTA, 0.0210 M"2000-

Untreated soil, No. 10 No. 60 FinesMin./Max. Values

Figure 5-10. Pesses: Total Cu concentrations in washed soil fractions.

5-12

RR3Q2633

TABLE 5-5. PERCENTAGE REDUCTION OF LEAD CONCENTRATIONSFROM THE UNTREATED SOIL

Site

Old Man's Township

C&R

Schuylkill

Gould soil

Gould casings

J&L Fabricating

Wash solution

WaterSurfactantEDTA

WaterSurfactant'EDTA

WaterSurfactantEDTA

WaterSurfactantEDTA

WaterSurfactantEDTA

Water .EDTA, 0.0084 M*EDTA, 0.0126 M*EDTA, 0.0168 M?EDTA, 0.0168 MD

No. 10

-219-104-148

26.72.78

-140

81.066.498.1

-13.67.21

67.5

82.978.879.7

-54.7-80.7-21674.2-17.0

No. 60

53.533.348.9

23.727.416.2

54.062.750.2

" 53.660.368.6

-

51.867.335.263.969.5

Fines

4.3824.114.1

27.623.864.7

37.343.715.0

-50.0-18944.7

34.149.044.3

-227-47.7-59.0-11.9-17.8

a pH = 7-8b pH = 11-12

5-13

263**

TABLE 5-6. PERCENTAGE REDUCTION OF METAL CONCENTRATIONSFROM THE UNTREATED PESSES SOIL

Metal

Lead

Cadmium

Nickel

Copper

Solution

WaterEDTA, 0.0106 M*EDTA, 0.0148 M^EDTA, 0.0210 M?EDTA, 0.0210 MD

WaterEDTA, 0.0106 MrEDTA, 0.0148 M*EDTA, 0.0210 M?EDTA, 0.0210 M°

WaterEDTA, 0.0106 M*EDTA, 0.0148 M°EDTA, 0.0210 M*EDTA, 0.0210 MD

WaterEDTA, 0.0106 M^EDTA, 0.0148 M*EDTA, 0.0210 M*EDTA, 0.0210 MD

No. 10

84.692.592.689.190.5

69.648.827.882.280.7

86.761.481.662.2

-232

93.495.993.892.394.1

No. 60

-15.110.7

-38.0-50.6-10.7

2.24-119-12.2-0.1

-59.8

-211-233-406-262-188

-55.8-15.3

-108.-100

-80.2

Fines

59.059.470.773.167.0

44.136.944.156.252. S

33.423.9-9.1647.445.6

72. 765.878.380.376.5

* pH - 7-8b pH « 11-12

5-14

8R302635

should be taller than those_for the surfactant and chelate washes. This isnot generally the case," however. For example, the soils from the Old Man'sTownship site showed more lead in the No. 10 fraction (coarse material) thanthe other fractions, and the lead in the large fraction from the chelate washshowed the highest concentration within the C&R soil fractions.

In most Bases', aTTThree wash solutions provided the same qualitativeresults for a given soil. For the'Old Man's Township soil (Figure 5-1), forexample, the lead concentrations in the No. 10 fractions are significantlygreater than those in the untreated soil. Concentrations in No. 60 fractionsare about the same or somewhat less than those in the untreated soil, andconcentrations in the fines are about the same. This may indicate that themechanical agitation and scrubbing of small particles from larger particlesis a more important variable than the wash solutions used for removal of leadfrom different sized particles.. For all soils except that from Pesses, leadconcentrations are qualitatively about the same or greater in the finefraction compared with those in the raw soil; about the same or less in theNo. 60 fraction; and from less to greater in the No. 10 fraction. TheSchuylkill and Gould battery casing samples indicate a distribution of leadin which the lead is concentrated in the fines, as is normally encountered insoil wasfvfng experiments.

The Old Man's township soil is the only soil for which the total leadconcentrations are consistently greater for the No. 10 fraction than for thewhole, untreated soil. During the experiments, the researchers noted thatthis soil often consisted of thick layers of clay surrounding larger par-ticles of gravel, The. layers of clay frequently were not rnechanically re-moved during the washing processes, and were only removed during rinsing andsieving. Thus, clay particles contaminated^with lead may have remained on the>2 mm soil fraction and contributed to the high total lead concentration. Asshown in Table 5-1, the Old Man's Township so.il contains a high percentage ofclay particles. - ---'" ".:•"".: —~-~ :•.-•—:.:.'-:. -.:.:::"- •.-_;•:—.::"""-" "—- -

Results for the Pesses soil differ from those for the other soils.Metal concentrations in the_No. 10_fractip_n__are._co_n.sistently less than in theraw soil, concentrations in the No. 60 fraction are consistently greater, andconcentrations in the fines are consistently smaller. These results are thesame regardless of "the metal or the wash solution, which again points tomechanical scrubbing as the primary method for lead removal.

Table 5-7 presents a summary of the percentage lead recovered in eachsoil fraction for all samples except "those from Pesses. The distributionamong the soil fractions has been adjusted_tp add up to 100 percent by divid-ing the amount of lead"determined to be in a particular fraction by the totalamount recovered in all fractions. The results are the same regardless ofthe starting soil concentration and, therefore, independent of the analyticalvariability in the starting soil. These results are shown graphically inFigures 5-11 through 5-16. The values for the Pesses soil are shown in Table5-8 and Figures 5-17 through 5-20.

5-15

SR302636

TABLE 5-7. PERCENT OF LEAD RECOVEREDIN WASH FILTRATE AND SOIL FRACTIONS

Site

Old Man'sTownship

C&R

Schuylkill

Gould soil

Solution

WaterSurfactantEDTA

WaterSurfactantEDTA

WaterSurfactantEDTA

WaterSurfactantEDTA

Gould casings Water

Site Solution

J&L WaterFabri- EDTA, 0.

SurfactantEDTA

Washfiltrate

a 0.070084M? 41.0

eating EDTA, 0.0126M? 36.4EDTA, 0.EDTA, 0.

0168Mr 58.10168MD 53.0

Washfiltrate

0.023.723.5

0.00.313.8

0.114.518.4

0.034.421.3

0.013.71.7

Rinse 1

0.048.64.110.37.4

No.10

32.120.417.6

32.736.346.3

7.810.12.9

27.813.0.3.3

18.518.025.1

Rinse 2

0.050.40.20.80.4

No.60

23.636.323.1

27.627.422.8

30.823.622.2

37.932.447.1__—** ™

No.10

21.618.924.82.712.3

Fines

44.439.635.9

39.636.117.0

61.351.856.5

34.250.122.3

81.578.273.2

No.60 Fines

26.4 51.713.4 17.620.1 14.214.9 13.312.6 14.1

pH * 7-8b pH = 11-12

5-16

ftR302637

Wash filtrate___ No. 10

Water runs Surfactant runs EDTA runs

Figure 5-11. Old Man's Township: Pb distribution after washing.

No. 10

Water runs Surfactant runs EDTA runs

Figure 5-12. C&R: Pb distribution after washing.

5-17

HR302638

Wash filtrateNo. 10No. 60.Fines

Watc- runs Surfactant runs EDTA runs

figure 5-13. Schuylkill: Pb distribution after washing.

fi~ 6oi ^ ^ m W///J7////////A imrfifflm i ^

Fines

Bgure 5-14. Gould soil: Pb distribution after washing.

5-18

SR302639

120

100-

£ »••**

§ 601£ -

40-

20-

120

Wash filtrateNo. 10Fines

Water runs Surfactant runs EDTA runs

Figure 5-15. Gould casings: Pb distribution after washing.

• Wash filtrateQ Rinse 1B Rinse 2E3 No. 10D No. 60• Fines

*pH = 11-12Water 0.0084 M 0.0126 M 0.0168 M 0.0168 M*

EDTA

Figure 5-16. J&L Fabricating: Pb distribution after washing.

5-19

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fiR3026Ul

120

100-

ej->1 60-j

40-

0

120

20-^ ^ ^ ^ ^ H ^ ^ ^ ^ ^ H ^ ^ ^ ^ ^ H ^ ^ ^ ^ ^ H

*pH = 11-12

Wash filtrateRinse 1Rinse 2No. 10

D No. 60• Fines

Water 0.0106 M 0.0148 M 0.0210 M 0.0210 M*

EDTA

Figure 5-17, Pesses: Pb distribution after washing.

• Wash filtrate@ Rinse 113 Rinse 2 .0 No. 10D No. 60• Fines

*pH = 11-12uWater 0.0106 M 0.0148 M 0.0210 M 0.0210 M*

EDTA

-18. Pesses: Cd distribution after washing.

5-21

z

d

120

100-i

40-

0

60 "l ra No. 10

120

100-

80-

40-

0

20-1= 11-12

'//SS///SSSSS/.

Wash filtrateRinse 1Rinse 2No. 10

D No. 60Fines

M Rinse 260 ~> El No. 10

D No. 60

Water 0.0106 M 0.0148 M 0.0210 M 0.0210 M*

EDTA

Figure 5-19. Pesses: Ni distribution after washing.

20-*pH = 11-12

Wash filtrateRinsel

Fines

Water 0.0106 M 0.0148 M 0.0210 M 0.0210 M"

EDTA

Rgure 5-20. Pesses: Cu distribution after washing.

5-22

SR3026W

As shown in Figures 5-11 through 5-207'almost Ho lead is recovered Inthe.wash filtrate for the water wash. The Tack of aqueous solubility of leadjustifies the use of the water wash as a control. For each of the soilfractions, the removal effictencfy resulting from the surfactant and EDTAwashes can therefore be calculated by comparison with the soil fractions fromthe water wash. These efficiencies are presented in Tables 5-9 and 5-10.Negative numbers indicate that the.concentration of lead in a particular soilfraction after the surfactant or EDTA wash was higher than that after thewater wash. The data do not indicate any obvious trends; the concentrationof any fraction actually should not increase in the surfactant or EDTAwashes. If any lead is removed at all (compared with the water wash), somelead would be expected to be removed from each of the soil fractions. Thedata indicate* again, that mechanical considerations may be more importantfor lead removal from soil fractions than the wash solution. Comparison ofTables 5-5 and 5-9 also shows the importance of mechanical action. In manycases in Table 5-5, the results show a reduction of lead in one soilfraction, but Table 5-9 shows that the reduction for the surfactant and EDTAis no greater than for water.

Lead Concentrations in Wash Solutions

The data discussed so far seem to indicate that soil washing was ineffec-tive in the significant removal of lead from the"soils or battery casingsunder consideration, and that mechanical agitation plays as great a role asthe wash solution. The removal efficiencies were found to be low, non-existent, or even negative when compared with the water control. Anothermeasure of the removal efficiency, however, is the amount of lead solubilizedin the wash medium during testing; because obtaining a representative sampleis easier and analytical precision is greater for a liquid than for a solid,the resulting data may be more definitive.

The data for the lead concentrations in the wash solutions are tabulatedagain in Tables 5-11 and 5-12. This information was also presented graphical-ly in Figures 5-11 through 5-20, in which the solid black area represents thefraction of solubilized lead (or solubilized metals for the Pesses soil)contained in the wash solution. The percentages given in these figures arethe amount of metals solubilized in the wash media and therefore representthe overall removal rate for the washing process. In all cases, thesurfactant and EDTA solutions solubilized much more lead than did water; forall the soils, the EDTA solution solubilized more than did the surfactant(the Pesses and J&L Fabricating soils were not tested with the surfactantwash). The chelate was significantly more effective than the surfactant forthe Old Man's Township, C&R, and Gould soils; the surfactant and EDTAefficiencies were of the same order of magnitude for the Schuylkill soil.For the battery casings, the surfactant removed a higher percentage of leadthan did the EDTA even though both removal rates are the same order of magni-tude. The surfactant solution worked best on soil at the Schuylkill site(14.5 percent removal) and worst on soil at the C&R site (0.28 percentremoval). The EDTA solution achieved 13.8 to 23.5 percent lead removal fromthe soils, but only 1.7 percent removal from the Gould battery casings. TheEDTA was also effective in chelating cadmium; as high as 21.6 percent was

5-23

SR3026UU

TABLE 5-9. PERCENTAGE REMOVALS OF TOTAL LEAD AS COMPARED WITHCONTROL (WATER WASH)

Old Man'sTownship

C&R

Schuylkill

Gould soil

Gould casings

O&L Fabri-cating

SurfactantEDTA

SurfactantEDTA

SurfactantEDTA

SurfactantEDTA

SurfactantEDTA

EDTA, 0.0084M*EDTA, 0.0126M*EDTA, 0.0168MEDTA, 0.0168M0

No. 10

35.922.2

-32.6-227.4

-77.00.7

18.371.4

-24.1-19.0

-16.8-10.483.324.4

No. 60

-86.0-10.1

17.0-9,9

51.5-8.3

19.532.3

—

32.1-34.525.036.7

Fines

20.610.1

-5.251.2

10.3-35.5

92.463.2

22.615.4

54.851.365.763.9

a pH * 7-8b pH = 11-12

5-24

aR3026lt5

TABLE 5-10. PESSES: PERCENTAGE REMOVALS OF TOTAL METALSAS COMPARED WITH CONTROL (WATERWASH)

Metal Wash solution No. 10 No. 60 Fines

Lead

Cadmium

Copper

Nickel

EDTA, 0.0106M*EDTA, 0.0148M;EDTA, O.Q210M?EDTA, 0.0210M0

EDTA, 0.0106M*EDTA, 0.0148M*EDTA, 0.021 OH?EDTA, 0.0210M

EDTA, 0.0106M*EDTA, 0.0148M*EDTA, Q.Q21QM*EDTA, 0.0210M0

EDTA, 0.01Q6M*EDTA, 0.0148M*EDTA, 0.021QM*EDTA, 0.0210M0

51.751.929.438.3

-68.5-138

41.336.5

38.26.7

-16.411.6

-189-38.3

-183-2391

22.4-19.9-30.83.8

-175. -41.0

-25.8-101

26.0-33.2-28.5-15.7

-7.1-62.9-16.67.2

0.9028.534.3

. 19.5

-12.90.021.615.7

-25.120.528.013.9

-14.2%-63.821.218.4

9 pH = 7-8b pH = 11-12

5-25

TABLE 5-11. PERCENTAGE OF LEAD RECOVERED IN WASH SOLUTION

WaterSurfactantEDTA

Old Man'sTownship C&R

0.02 03.7 0.2823.5 13.8

Schuylkill Gould soil

0.13 0.0314.5 4.418.4 21.3

Gould casings

0.013.71.7

ILCO

WaterEDTA, 0.0084M*EDTA, 0.0126M,EDTA, 0.0168M*EDTA, 0.0168M0

0.07341.036.458.153.0

a pH = 7-8b pH = 11-12

TABLE 5-12. PERCENTAGE OF METALS RECOVERED IN WASH SOLUTIONFOR THE PESSES SITE

WaterEDTA, O.Q1Q6M*EDTA, O.Q148M*EDTA, 0.0210M?EDTA, 0.0210M0

Lead

020.721.923.223.2

Cadmi urn

0.1910.114.821.618.0

Copper

0.03.9.056.727.966.03

Nickel

0.191.821.602.030.86

a pH = 7-8b pH * 11-12

5-26

SR30261*?

solubilized from the Pesses soil. The EDTA was less effective on copper andnickel; a maximum of 9.05 percent copper and 2.03 percent nickel were solubi-lized from the soil.

During the soil washing experiments, EDTA was added at a 3:1 molar ratiobased on the total amount of chelatable metals in the soil, including lead,calcium, iron, and others. The J&L Fabricating and Pesses soils were treatedwith three different concentrations of EDTA and.at two pH values. Tables5-13 and 5-14 present the volume of Versene 100 added to each wash solutionand the resulting molar concentration of EDTA. One gram of Versene 100,which is 39 weight percent EDTA, will chelate approximately 1 millimole ofmost metal ions. Thus, the maximum concentration of lead chelated by EDTA inthe wash solution can be determined by the following formula:

elation - 100)

x Hoi. wght. Pb

For example, a 3:1 molar ratio would result in a maximum chelation efficiencyof (0.33 mole Pb/mole EDTA) x ( M W / M W ^ x 100% = 18 Percent-

The chelation efficiency results are given in Tables 5-13 and 5-14.Finally, the percent of EDTA that has chelated with the lead can becalculated by dividing the lead concentration by the maximum chelation oflead; this value indicates the EDTA chelation efficiency. These values donot account for other chelatable metal ions present or the concentration oflead in the soil available for chelation.

Several of the results indicated in Table 5-13 are important. As theconcentration of EDTA increases for the Schuylkill, Gould, Old Man's Town-ship, and C&R soils, the lead concentration in the wash solution generallyincreases. This same trend is apparent for the three molar concentrationsused in treating the.ILCO soil and for metal concentrations for the Pessessoil. The percentage "of maximum chelatioh achieved for the Schuylkill,Gould, Old Man's Township, and C&R sites, however, are the same order ofmagnitude, ranging from 3.6 to 7.5 percent. The maximum chelation achievedfor the J&L Fabricating site ranged from 13 to 19 percent, and the higherEDTA concentrations resulted in lower efficiencies. The chelationefficiencies for the Pesses site averaged 0.39 percent for lead, 3.8 percentfor cadmium, 1.7 percent for nickel, and 5.7 percent for copper. The Gouldbattery casings showed a very low chelation efficiency — 0.17 percent. Theamount of lead solubilized is not dependent on particle-size distribution orlead speciation.

Results for the O&L Fabricating and Pesses soils show that although themetal concentrations or the wash filtrates increase with increasing EDTAconcentrations, the chelation efficiency decreases. The low-lead chelation

5-27

R3026U8

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flR302650

efficiencies for the Pesses site are probably due to low concentrations oflead in the soil.

The results for the J&L Fabricating soil indicate that the chelationefficiencies for the Old Man's Township, C&R, Schuylkill, and Gould soils areprobably not the best that can be achieved; i.e., increasing the aggressive-ness of the test conditions could increase the chelation efficiency andresult in higher lead concentrations in the wash solution and thereforehigher removal efficiencies from the soil. During the soil washing testsconducted on the G&L Fabricating and Pesses soils, some of the glass labora-tory equipment broke on the reciprocating shaker. The number of vibrationsper minute was therefore decreased during the tests on the other four soilsand the battery casings, which resulted in less suspended solids and lesscontact between the liquid and solid phases. For this reason, the system maynot have been at equilibrium when the mixing was stopped. Increasing theagitation and contact time probably could increase the chelation efficiency.Results for the battery casings support this conclusion; the low chelationefficiency may be due to lead being trapped within the rubber particles,which were too heavy to be suspended in solution.

The soil washing data collected in these experiments are not dependenton particle-size distribution or mineralogy. The important variables wereextent of agitation, starting lead concentration, and EDTA concentration.

TCLP data

In the remediation of a Superfund site, cleanup goals may be expressedin terms of removal efficiency or the reduction of the mobility of toxicmaterials. Therefore, TCLP extractions were conducted on all soil fractionsfrom the Gould site and all soil fractions resulting from the EDTA wash (thislimited test program was due to cost constraints). Table 5-15 presents re-sults from TCLP testing of the Gould soil fractions; TCLP results for the rawsoils are also included for comparison. Table 5-16 presents comparable datafor the EDTA wash. TCLP and EP toxicity extractions were conducted on theO&L Fabricating and Pesses sites; these results are presented in Tables 5-17through 5-20. These tables also present the percentage reductions of theTCLP data on the soil fractions compared with the raw soil.

None of the soil fractions (except Pesses) achieved the 5 mg/L criterionfor the TCLP extract. However, some soil fractions may meet or approachless-stringent cleanup criteria (such as 40 mg/L) that have been proposed forsome sites. None of the Pesses soil fractions achieved the 1 mg/L criterionfor cadmium. A comparison of the percentage reduction in TCLP data on thesoil fractions with that in the raw soil indicates that significant reductionsin TCLP extraction lead concentrations were achieved over those in the rawsoil, even when total lead concentrations were not decreased. This findingindicates that the wash process removes a proportionally greater percentageof lead that is also leachable under the conditions of the TCLP. The waterwash also achieved significant reductions in TCLP leachable lead, except forthe fines. This result lends support to the hypothesis that much of the leadremoval Is due to mechanical agitation and scrubbing of the soil particles.

5-30

AR302651

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Summary of Results

The soil washing results indicate that although the removal efficienciesbased on residual soil concentrations were disappointing and conflicting, theremoval efficiencies based on lead concentrations in the wash media indicatethat lead is solubilized to a significant extent in the surfactant and EDTAsolutions. The 5 mg/L criterion for lead was not achieved in the TCLPextracts; however, nearly all TCLP values were lower than those of the rawsoil, which indicates that much of the TCLP-leachable lead is removed duringsoil washing. Mechanical agitation was an important variable for leadremoval. The results were not dependent on particle-size distribution orlead speciation. Because the tests were conducted under only one set ofconditions, it Is impossible to determine whether the wash system was atequilibrium and that the preceding results are the best that can be achieved,or if a longer "contact time "between the soil and wash solutions would haveresulted in increased solubilization and chelation efficiency and, therefore,higher removal. Neither do the _data indicate whether other conditions suchas an increased liquid-to-sol id ratio, increased concentrations of surfactantor EDTA, more agitation, multiple wash steps, different pH's, heatedsolutions, or crushing soils before washing would have increased lead removalefficiencies. - T - •

5.3 SOLIDIFICATION/STABILIZATION

Solidification/stabilization tests were conducted on the fine fractions(< 2mm) of soil from the Gould site after soil washing. Table 5-21 lists thedata that were collected on the fine fractions prior to solidification.

TABLE 5-21. CHARACTERIZATION OF THE GOULD FINESAFTER WASHING

Parameters A B Average

PHMoisture content [To be filled in when data are available]Humic acid • - - - . . - . . . . . -Particle-size analysisTotal leadTCLP leachable lead

The soil washing residuals, resulting from washing the Gould site soilwith water, surfactant, and chelate, were mixed individually with a solidi-fication agent (portlant cement) to evaluate the effect of a cement-based S/Sprocess on the immobilization of the lead in the soil fraction consisting ofparticles <2 mm in diameter. The material was mixed at a cement-to-soilratio of 0.25 and a water-to-total-solids ratio of 0.4. After a 14-day

5-35

SR302656

curing period, the solidified product (crushed and monolithic) plus an un-solidified sample were subject to the monofilled waste extraction procedure(MWEP); the extracts were measured for pH and analyzed for total lead. Theresults are presented in Table 5-22.

(Insert Discussion Results Here]

5.4 QUALITY ASSURANCE

The quality assurance results for total lead analysis are presented inTable 5-23. The QA objectives for accuracy were 75 to 125 percent and lessthan 20 percent relative difference (RPD) for precision. Only one of sixsolid samples for the Old Man's Township, C&R, Schuylkill, and Gould sitesachieved these objectives, whereas all of the liquid samples met the objec-tives. The percentage recovery for the No. 10 soil fraction was always low,whereas the percentage recovery for the No. 60 soil fraction was usuallyhigh. Therefore, the QA objectives were generally achieved for the fine soilfraction. Six of the 12 QA objectives were achieved for the J&L Fabricatingsoil, and the majority of the Pesses samples achieved the QA objectives.(The Pesses soil samples that were out of range were reanalyzed; therefore,the specific QA results for Pesses have not been presented.) Differences inthe recoveries of the matrix spike/matrix spike duplicates in the soil samplesare attributed to difficulties in obtaining a representative sample foranalysis because of the very small volume (about 1 gram) required.

In additional to replication of analytical results by conducting matrixspike duplicates, the wash process itself was conducted in duplicate runs.The resulting duplicate data points indicate the precision of the experimentaldesign. Table 5-24 presents the average RPDs between the two runs conductedunder each test condition for the second test series (i.e., for the Old Man'sTownship, CSR, Schuylkill, and Gould soils). Values are given for weights,lead concentrations in each medium, and the percentage of lead in each medium.In addition, an overall average of the RPD is given on the right-hand side ofthe table for each parameter.

The RPD for the weight data fall within 20 percent precision; all theoverall average RPO data are less than or equal to 15 percent. The 15 per-cent value was obtained from the amount collected on the filter paper, whichcould vary depending on how much solution was filtered and how often thefilters were changed. The lead concentration values vary widely, with severalRPDs greater than fifty percent. The overall average data indicate that leadconcentrations for the No. 10 soil are the least precise (64%) followed bythe Ho. 60 soil fraction with a 46 percent RPD. These results were as expect-ed qualitatively because of the difficulty in obtaining a representativesample of larger particles. All of the average values are, however, outsidethe goal of a 20 percent RPD. The total lead recovered had an RPD of 15.

5-36

UR302657

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5-37

R302658

TABLE 5-23. QA/QC RESULTS FOR SOIL WASHING

Site

SchuylkillSchuylkillSchuylkillSchuylkillSchuylkillSchuylkillC5ROld Man'sTownshipGouldJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L FabricatingJ&L Fabricating

Washsolution

WaterWaterSurfactantSurfactantEDTAEDTAWaterEDTA

WaterWaterEDTA, 0.0084 MEDTA, 0.0126 MEDTA, 0.0168 M,EDTA, 0.0168 MDWaterEDTA, 0.0084EDTA, 0.0126 MEDTA, 0.0168 MEDTA, 0.0168 MEDTA, 0.0168 MEDTA, 0.016S H

Matrix

No. 10 soilNo. 60 soilNo. 10 soilNo. 60 soilNo. 60 soilFinesWashWash

WashFinesFinesFinesFinesFinesRinse 2Rinse 2Rinse 1WashWashFinesFines

Percentrecovery(accuracy)MS MSD

64107.357.9173.519110299.098.1

91.2110

" 57.999.611062.910411156.052.019.017082.4

55.1156.747.978.2142 .94.199.1108.0

90.710478.367.694.652.510811816.648,010.014974.7

Precision,RPD

14.937.418.975.729.48.060.1C19.61

0.5505.630.038.315.118.03.86.1

1088.0

62.113.29.S

5-38

flR302659

TABLE 5-24. RELATIVE PERCENT DIFFERENCE FOR DUPLICATE RUNS

Average RED for " Overall averagesoils3 RPD

Weights

No. 10No. 60PanFilterFines ~ _:::Total collected

Water

7.87.05.59.5.8

- 3.7

Surfactant

152.55.519101.4

EDTA

U5.714175.92.0

11 _5.18.3156.62.4

Pb concentration

Wash solutionNo. 10No. 60Fines ----- — —Total Pbrecovered

5370.56

~ 3121 '

12. 78

523216

Percent Pb in each

Wash solutionNo. 10No. 60Fines

71544548

25634542

17432.9208.6

medium

. 10 _.463014

2764462815

35544035

5-39

HR302660

As expected, the percentage of lead in each medium indicate the sametrends as the lead concentrations themselves. The adjusted percentage forthe No. 10 soil is the least precise, followed by the No. 60 soil, and thenby the fines and wash solution.

A total of five QA/QC checks were performed on the TCLP results for thesecond test series by using the four-point method of additions. All samplesfell within the 20 percent objective for precision.

5-40

AR3Q266!

APPENDIX A

STANDARD OPERATING PROCEDURES

A-l

R302662

STANDARD OPERATING PROCEDURE

BATTERY CASING WASHING PROCESS

The battery casing washing procedure, shown schematically in Figure 1,is outlined below.

1. Prepare 5000 ml of the wash solution in a 10-liter, widemouth glass jar.In this study, three wash solutions were evaluated:a. Tap water, pH=7

b. EDTA (3:1 molar ratio of EDTA to lead content of untreated material)(adjust the pH of the chelate wash solution to between 7-8)

Dc. 0.5 percent by weight surfactant (Tide )

Record the temperature and pH of the solution.

2. If necessary, prescreen the battery casings to remove large scrapmaterial, such as debris, cobble, etc.

3. Shred the battery casings in a laboratory mill. Place the outletmaterial on a 3/8-in. wire mesh sieve stacked on a bottom receiving pan.Place a cover on the sieve and shake the sieve stack on a sieve shakerfor 5 minutes. Recycle the oversized material (retained on the sieve)to the mill,

4. Weigh out 500 g of the shredded battery casings on a triple-beam balanceand place in the jar containing the wash solution. (The liquid-to-solidweight ratio should be 10:1.) Place the jar on a reciprocating shakerand agitate vigorously for 30 minutes.

5. Empty the contents of the jar onto 110 wire mesh sieve stacked on abottom receiving pan that has been fitted with a side drain (1/4-in.-dia-meter pipe connected to a 3-ft length of tygon tubing). Drain theliquid and sludge into a large polyethylene bucket.

6. Place a cover on the sieve and shake the sieve stack on a sieve shakerfor 10 minutes to aid separation of the rubber particles.

A-2

AR3Q2663

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7. Pressure filter the slurry in the bucket from Step 4 under 40 psipressure. Collect a representative sample of the filtrate in an 8-ozglass jar for analysis; discard the remaining filtrate.'"

8. Measure the pH and temperature of the filtrate.

9. Using nitric acid, preserve the filtrate by adjusting the pH between 1and 2.

10. Using a hand-held sprayer, rinse the rubber on the sieve with 1000 ml ofwater. Place cover on the sieve and shake the sieve stack on a sieveshaker for 10 minutes. Repeat the rinse and sieve shake steps. Weighthe rubber and collect a representative sample into 8-oz glass jars foranalysis. Save the rinsate for Step 11.

11. Rinse the filter cake in the pressure-filter apparatus with 2000 ml ofthe rinsate from Step 10. Weigh the filter cake and the fines remaininginside the pan and collect a representative sample for analysis.Discard the rinsate.

12. Decontaminate all equipment and glassware by washing with a standardlaboratory detergent and then rinsing with nitric acid and deionizedwater.

A-4

STANDARD OPERATING PROCEDURE

SOIL WASHING PROCESS

The soil washing procedure, shown schematically in Figure 2, is outlinedbelow. .

1. Prepare 5000 ml of the wash solution in a 10-liter, widemouth glass jar.In this study, three wash solutions were evaluated:a. Tap water, pHs7

b. EDTA (3:1 molar ratio of EDTA to toxic metals), (adjust the pH ofthe chelate wash solution to between 7-8)

Dc, 0.5 percent by weight surfactant (Tide )

Record the temperature and pH of the solution. For Pesses and ILCOsites only, adjust the pH of the surfactant wash solutions to between 7-8 byusing sulfuric acid and measure the volume of acid added.

2. If necessary, prescreen the soil to remove large scrap material, such asdebris, cobble, etc.

3. Weigh out 500 g of soil on triple-beam balance and place in the jarconatining the wash solution. (The liquid-to-solid weight ratio shouldbe 10:1) Place the jar on a reciprocating shaker and agitate vigorouslyf o r 3 0 minutes. • • - - . . . . . .

4. Stack a #10 and a #60 wire mesh sieve on a bottom receiving pan that hasbeen fitted with a side drain (1/4-in.-diameter pipe connected to a 3-ftlength.of tygon tubing). Empty the contents of the jar onto the sievestack. Drain the liquid and fines into a large poloythylene bucket.

5. Place cover on the top sieve and shake the sieve stack on a sieve shakerfor 10 minutes to aid separation of the soil particles.

A-5

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A-6

flR302667

6. Pressure filter the slurry in the bucket from Step 4 under 40 psipressure. Collect a representative sample of the filtrate in an S-ozglass jar for analysis; discard the remaining filtrate.

7. Measure the pH and temperature of the filtrate.

8. Using nitric acid, preserve the filtrate by adjusting the pH between 1and 2.

9. Using a hand-held sprayer, rinse the soil on the #10 sieve with 1000 mlof water. Remove the top sieve and rinse the soil on the #60 sieve with1000 ml of water. Replace the top sieve, cover, and shake the sievestack on a sieve shaker for 10 minutes. Repeat the rinse and sieveshake steps. Save the rinsate for Step 11.

10. Weigh the two soil fractions retained on the sieves (No. 10 and No. 60)and collect representative sample into two separate 8-02 glass jars foranalysis.

11. Rinse the filter cake in the pressure-filter apparatus with 2000 ml ofthe rinsate from Step 9. Weigh the filter cake and the fines remaininginside the pan and collect a representative sample for analysis.Discard the rinsate.

12. Decontaminate all equipment and glassware by washing with a standardlaboratory detergent and then rinsing with nitric acid and deionizedwater.

A-7

ftR302668

STANDARD OPERATING PROCEDUREFOR SOLIDIFICATION/STABILIZATION

OF SOIL SAMPLES

Proposed outline for further treatment (Stabilization/Solidification) ofthe fines (<2mm) from the Gould site is as follows:

1. Place 2.3kg of the fines (<2mm) from the soil washing experimentinto a plastic pan, and mix thoroughly for 10 minutes.

2. Select 3 random samples of the soil from step 1. These samples willbe used to measure the moisture content of the waste material.Results cf the moisture content tests are required to determine theweight of the soil and water that is needed for the preparation ofthe S/S specimens.

3. If the average moisture content of the soil is greater than 25percent, dewater the sample until the moisture content is less thanor equal to the threshold value.

4. Collect replicate samples of the soil for analysis of pH, moisturecontent, humic acid, total lead content, particle size analysis andTCLP.

^ ih 20 grams of the portland cement (type 1) and mix it with halft- :he water required for preparation of the S/S specimen.

6. Add 80 grams of the soil (on a dry weight basis) to the cement-watermixture provided in step 5, and hand mix the material thoroughlyfor 10 minutes.

7. Add the remaining half of the water to the mixture and blend thematerial until a workable mix is achieved. The cement to dry soil

A-8

AR302669

ratio (W/W) is 0.25 and the water to total solids ratio is 0.4. For80 grams of dry soil, this corresponds to 20 grams of cement and 40grams of water.

8. Fill preweighed cylindrical molds with approximately 125 grams ofthe mixture.

9. Seal the molds with teflon caps and allow the samples to cure in amoist room for 14 days. The room should have a temperature of72°F ± 5°F with a 100 percent relative humidity.

10, Remove the solidified samples from their molds and crush themseparately so that the crushed particles can pass through a 9.5 mmstandard sieve (crushing of the samples is required for the TCLPtest).

11. Collect 6 of the crushed samples for the TCLP test.

A-9

AR3026

STANDARD OPERATING PROCEDURE

BATTERY CASING LEACHINGBUREAU OF MINES PROCESS

The proposed battery casing leaching procedure, shown schematically inFigure 1, is outlined below.

1. Prepare x ml of an ammoniacal leaching solution consisting of x wt. %ammonium carbonate and x wt. % ammonium bisulfite. Record the pH of thesolution.

2. Prepare x ml of an x wt. % solution of fluosilicic acid. Record the pHof the solution.

3. If necessary, prescreen the battery casings to remove large scrapmaterial.

4. Shred the battery casings in a laboratory mill. Place the outlet mauon a 3/8-in. wire mesh sieve stacked on a bottom receiving pan. Place acover on the sieve and shake the sieve stack on a sieve shaker for 5minutes. Recycle the oversized material (retained on the sieve) to themill.

5. Place the ammoniacal leaching solution into a 10-liter, widemouth glassjar. Insert a heating element into the jar through the lid. Heat thesolution to 55°C; adjust the volatage of the heating element to maintainthe temperature at 55°C.

6. When the temperature of the solution reaches steady state, weigh out x gof the shredded battery casings on a triple-beam balance and place inthe jar. (The liquid-to-solid weight ration should be x:l). Place thejar on a reciprocating shaker and agitate vigorously for 1 hour. Record

A-10

flR30267i

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A-ll

R302672

the temperature every 15 minutes and adjust the voltage of the heatingelement as necessary.

7. Empty the contents of the jar onto a #10 wire mesh sieve stacked on abottom receiving pan that has been fitted with a side drain (1/4-in.-diameter pipe connected to a 3-ft length of tygon tubing). Drain theliquid and sludge into a large polyethylene bucket.

8. Place a cover on the sieve and shake the sieve stack on a sieve shakerfor 10 minutes to aid separation of the rubber particles.

9. Pressure filter the slurry in the bucket from Step 7. Collect a repre-sentative sample of the filtrate of analysis; discard the remainingfiltrate.

10. Using a hand-held sprayer, rinse the rubber on the sieve with x ml ofwater. Place a cover on the sieve and shake the sieve stack on a sieveshaker for 10 minutes. Repeat the rinse and sieve shake steps. Savethe rinsate for Step 17.

11. Weigh the rubber. Add an amount of the fluosilicic acid solution to a5-liter, widemouth glass jar so that the liquid-to-solid weight ratio is

12. Insert a heating element into the jar through the lid. Heat the solutionto 50°C; adjust the voltage of the heating element to maintain thetemperature at 50°C.

13. When the temperature of the solution reaches steady state, add therubber from Step 11 to the jar. Place the jar on a reciprocating shakerand agitate vigorously for 1 hour. Record the temperature every 15minutes and adjust the voltage of the heating element as necessary.

A-12SR3Q2673

14. Empty the contents of the jar onto a #10 wire mesh sieve stacked on abottom receiving pan that has been fitted with a side drain. Drain theliquid into a large polyethylene bucket.

15. Place a cover on the sieve and shake the sieve stack on a sieve shakerfor 10 minutes.

16. Using a hand-held sprayer, rinse the rubber on the sieve with x ml ofwater. Place a cover on the sieve and shake the sieve stack on a sieveshaker for 10 minutes. Repeat the rinse and sieve shake steps. Weighthe rubber and collect a representative sample for analysis. Save therinsate for Step 22.

17. Rinse the filter cake in the pressure-filter apparatus with x ml of therinsate from Step 10. Discard the rinsate.

18. Weight the filter cake. Add an amount of the fluosilicic acid solutionfrom Step 14 to a 5-liter, widemouth glass jar so that the liquid-to-solid ratio is x:l. . ...._ .

19. Insert a heating element into the jar through the lid. Heat the solu-tion to 50°C; adjust the voltage of the heating element to maintain thetemperature at 50°C.

20. When the temperature of the solution reaches steady state, add thefilter cake from Step 18 to the jar. Place the jar on a reciprocatingshaker and agitate vigorously for 1 hour. Record the -temperature every15 minutes and adjust the voltage of the heating element as necessary.

21. Pressure filter the slurry from Step 20. Collect a representativesample of the filtrate for analysis; discard the remaining filtrate.

A-13

22. Rinse the filter cake in the pressure-filter apparatus with x ml of therinsate from Step 16. Weigh the filter cake and collect a representa-tive sample for analysis. Discard the rinsate.

23. Decontaminate all equipment and glassware by washing with a standardlaboratory detergent and then rinsing with nitric acid and deionizedwater.

A-14

3R302675

STANDARD OPERATING PROCEDURESOIL LEACHING

— BUREAU OF MINES PROCESS

The proposed soil leaching procedure, shown schematically in Figure 2,is outlined below.

1. Prepare x ml of an ammoniacal leaching solution consisting of x wt. %ammonium carbonate and x wt. % ammonium bisulfite. Record the pH of thesolution.

2. Prepared x ml of .an x wt. % solution of fluosilicic acid. Record the pHof the solution.

3. If necessary," prescreen the soil to remove large scrap material.

4. Place the ammoniacal leaching solution into a 10-liter, widemouth glassjar. Insert a heating element into the jar through the lid. Heat theso-lution to 55°C; adjust the voltage of the heating element to maintainthe—temperature at 55°C.

5. When the temperature of the solution reaches steady state, weigh out x gof soil on a triple-beam balance and place in the jar. (The liquid-to-solid weight ratio should be x:l). Place the jar on a reciprocatingshaker and agitate vigorously for 1 hour. Record the temperature every15 minutes and adjust the voltage of the heating element as necessary.

6. Stack a #10 and a #60 wire mesh sieve on a bottom receiving pan that hasbeen fitted with a side drain (1.4-in.-diameter pipe connected to a 3-ftlength of tygon tubing. Empty the contents of the jar onto the sievestack. Drain the liquid and fines into a large polyethylene bucket.

7. Place a cover on the top sieve and shake the sieve stack on a sieveshaker for 10 minutes to aid separation of the soil particles.

A-15

flR302676

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A-16

SR302677

8. Pressure filter the slurry In the bucket from Step 6. Collect a repre-sentative sample of the filtrate for analysis; discard the remainingfiltrate.

9. Using a hand-rheld sprayer, rinse the soil on the #10 sieve with x ml ofwater. Remove the top sieve and rinse the soil on the #60 sieve with xml of water. Replace the top sieve, cover, and shake the sieve stack ona sieve shaker for 10 minutes. Repeat the rinse and sieve shake steps.Save the rinsate for Step 19.

10. Weigh the two soil fractions retained on the sieves. Add an amount ofthe fluosilicic acid solution to each of two 5-liter, widemouth glassjars so that the liquid-to-solid weight ratio is x:l.

11. Insert a heating element into each of the two jars through the lids,Heat the solutions to 50°C; adjust the voltages of the heating elementsto maintain the temperatures at 50°C.

12. When the temperatures of the solutions reach steady state, add the twosoil fractions from Step 10 to the respective jars. Place the jars on areciprocating shaker and agitate vigorously for 1 hour. Record thetemperatures every 15 minutes and adjust the voltages of the heatingelements as necessary.

13. Empty the contents of the jar containing the coarse soil fraction onto a#10 wire mesh sieve stacked on top of a bottom receiving pan that hasbeen fitted with a side drain. Drain the liquid into a large poly-ethylene bucket and save for Step 20.

14. Place a cover on the sieve and shake the sieve stack on a sieve shakerfor 10 minutes.

A-17

H r\ '"t f\ o f ~~j /•%$R302678

15. Empty the contents of the jar containing the medium soil fraction onto a160 wire mesh sieve stacked on top of a bottom receiving pan that hasbeen fitted with a side drain. Drain the liquid into the bucket fromStep 13 and save for Step 20.

16. Place a cover on the sieve and shake the sieve stack on a sieve shakerfor 10 minutes.

17. Using a hand-held sprayer, rinse the soil on the #10 sieve with x ml ofwater. Place a cover on the sieve and shake the sieve stack on a sieveshaker for 10 minutes. Repeat the rinse and sieve shake steps. Weighthe soil and collect a representative sample for analysis. Save therinsate for Step 24.

18, Using a hand-held sprayer, rinse the soil on the #60 sieve with x ml ofwater. Place a cover on the sieve and shake the sieve stack on a sieveshaker for 10 minutes. Repeat the rinse and sieve shake steps. Weightthe soil and collect a representative sample for analysis. Save therinsate for Step 24.

19. Rinse the filter cake in the pressure-filter apparatus with x ml of therinsate from Step 9. Discard the rinsate.

20. Weigh the filter cake. Add an amount of the combined fluosilicic acidsolutions from Steps 13 and 15 to a 5-liter, widemouth glass jar so thatthe llquid-to-solid ratio is x:l.

21. Insert a heating element into the jar through the lid. Heat the solu-tion to 50°C; adjust the voltage of the heating element to maintain thetemperature at 50°C.

22. When the temperature of the solution reaches steady state, add thefilter cake from Step 20 the the jar. Place the jar on a reciprocatingshaker and agitate vigorously for 1 hour. Record the temperature every15 minutes and adjust the voltage of the heating element as necessary.

A-18

AR3Q2679

23. Pressure filter the slurry from Step 22. Collect a representativesample of the filtrate for analysis;" discard the remaining filtrate.

24. Rinse the filter cake in the pressure-filter apparatus with x ml of thecombined rinsate from Steps 17 and 18. Weigh the filter cake andcollect a representative sample for analysis. Discard the rinsate.

25. Decontaminate all equipment and glassware by washing with a standardlaboratory detergent and then rinsing with nitric acid and deionizedwater.

A-19

flR302680

APPENDIX B

SOIL CHARACTERIZATION DATA

B-l

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R302&S1*

TABLE B-3. HUMIC ACID CONTENT

Humic acid, weight percent

Old Man's Township

C&R

SchuyUill

Gould

Gould battery casings

Control blank

A

0.390.42

0.000.02

0.770.84

1.691.35

0.020.02

0.04<0.01

B

0.350.22

0.060.07

0.770.67

0.741.06

0.330.16

0.03<0.01

Average

0.35

0.04

0.76

1.21

0.13

B-5

flR302685

TABLE B-4. WESTERN RESEARCH INSTITUTEMINERALOGIC ANALYSIS

Sample Mineral identification

Schuylkill quartz, calcite, cerussite*, smectite

Gould soil quartz, Na, Ca feldspar, anglesite, plattnerite,lead, smectite, illite

C&R quartz, calcite, hydrocerussite*, bassanite,plagioclase, illite, smectite

NL Industries ... quartz, calcite, cerussite*, bassanite, lead,illite, kaolinite •

Gould casing chips anglesite, plattnerite, lead, quartz, illite,smectite

C&R quartz, calcite, hydrocerussite*, bassanite,plagioclase, illite, smectite

Gould casings anglesite, plattnerite, lead, quartz, illite,smectite

Gould soil quartz, anorthite, anglesite, plattnerite, lead,smectite, illite

Old Man's Township quartz, calcite, cerussite*, bassanite, lead,illite, kaolinite

Schuylkill quartz, calcite, cerussite*, smectite

Mineral Code _ _ _ , . „ - _ „ . ^

quartz Si02 plattnerite Pb02calcite CaC03 * bassanite CaSO^.-SHaOplagioclase (Na,Ca)AlSi308 illite K-Al-Si-0-Hanorthite (Ca,NA]A"lSi309 smectite Na-Ca-Al-Si-0-Hanglesite PbSOi^ kaolinite A12SI205(OH)4cerussite PBC03 lead (metal) Pbhydrocerussite P*The XRD patterns and crystalline structures for the minerals cerussite andhydrocerussite are very similar and differ only in the degree of hydration.Additionally, the mineral leadhillite Pb^CSOMCOg^OH^ is very similarin structure to cerussite and hydrocerussite and differs by the substitutionof S04 into the crystalline form. It is very possible that leadhillite waspresent in some or all of the samples that contained cerussite or hydro-cerussite, but was masked by other peaks or below detection limits.

B-6

flR302686

TABLE B-5. SAMPLE CHARACTERIZATION RESULTSFOR O&L FABRICATING UNTREATED SOIL SAMPLES

Analyte

AluminumAntimonyArsenicBariumBeryl 1 i urnCadmi urnCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMercuryNickelPotassiumSeleniumSilverSod i urnThalliumVanadiumZincTOCCyanideFluoride, mg/gSulfateMoisture, %Na CEC, meq/100 gpH, S.U.

Concentration,

WestPile No. 1

17,60022368.6303

1.453.67

68,10014.3<1.40

20215,0004,51017,400

710<0.1212.6

1,680<0.18<1.14

1,390<29.427.9272

4,3440.510.87

3398.113.86.22

uq/q (except as

SmallPile No. 1

19,30013.273.0373

1.572.51

77,30014.7<1.42

. 12515,9003,38017,600

720<0.1210.9

1,780<0.18<1.14

1,430<29.628.0314

2,8330.781.71

2549.516.746.4

TABLE B-6. WEIGHT PERCENTAGE OF ILCO TREATED SOIL

Soil fraction

>2 mm0.25 to 2 mm<0.25 mm

Total

Wet weight

188740214

1142

indicated)

BigPile No. 4

12S400144299626

0.8613.4

37,40036.2<1.39454

62,20030,40010,300

6170.14

56.01,000

<0.98<1.44

1,060<28.020.3

- 1,4605,149

0.161.2

164147.756.55

FRACTIONS

, g Weight percent

166418

100

.5

.8

.7

.0

B-7

AR302687

TABLE B-7. SAMPLE CHARACTERIZATION RESULTS FOR PESSES UNTREATED SOIL

Concentration, ycj/g (except as

Analyte

AluminumAntimonyArsenicBariumBerylliumCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMercuryNickelPotassiumSeleniumSilverSodiumThalliumVanadiumZ-i ncTOC . -CyanideFluoride, mg/gSulfateMoisture, %Na CEC, meq/100pH, S.U.

01A

4,140<10.212.6

---"45- -<0.17

1,45087,500

151 .<1.49

2,19025,600

2298493357.93

1,630916<0.196.73

187<31.08.36

350

9

01B QIC

4,940<10.09.7845,7<0.18

1,55043,700

549<1.50 ...

6,32021,900

3757042498.72

1,4101,390

<0.193.92

302<31.410.5651

14,50017.41.25

- •-• - ~- — . . ---g;10.7313.46.55

noted)

Average

4,540<10.111.245.4<0.18

1,50065,600

350<1.50

4,26023,800

3027762928.32

1,5201,150

<0.195.32

244<31,29.43

50014,500

17.41.259710.7313.46.55

TABLE B-8 WEIGHT PERCENTAGE OF PESSESSOIL FRACTIONS

Soil fraction

>2 mm0.25 to 2 mm<0.25 mm

Total

Weight percentage

18.531.550.0

100.0

B-8

flR302688

APPENDIX C

RESULTS OF SOIL WASHING

C-2

TABLE C-l. RESULTS OF SOIL WASHING TESTS FOROLD MAN'S TOWNSHIP

Water

Weight, g

No. 10No. 60PanFilter

Pb concentration

Wash filtrateNo. 10No. 60Fines

A

9.4.0525.3193.8254.2

» mg/kg

0.3855,20027,30062,500

B

106.4485.8202.9273.9

for solids,

1.19251,00017,3002-9,300

Surfactant

A

95.4470.5207.3232.5

mg/L for 1

133143,00045,40033,700

B

79.5480.7195.6276.1

iquids

17453,20018,60039,200

EDTA

A

78.7499.6209.4269.4

1,360145,00027,30039,500

B

78.7504,2181.6268.5

1,15093,10021,80043,000

TABLE C-2. RESULTS OF SOIL WASHING TESTS FORC&R BATTERY SITE

Water .

Weight, g

No. 10No. 60PanFilter

Pb concentration

Wash filtrateNo. 10No. 60Fines

A

363.1276.3219.3216.4

, mg/kg

0.3130,20038,00053,400

B

340.0294.6186.6240.4

for solids,

. 0.1570,10066,40045,600

Surfactant

A

361.3317.4193.5169.3

mg/L for

-17.252,20050,04054,700

B

277.4327.7190.9256.6

liquids

15.880,80049,30049,500

EDTA

A

233.4187.7193.9267.4

1,350160,40052,90031 ,300

B

150.5354.9148.3351.4

533.0168,00061,80017,040

C-3

fiR302690

TABLE C-3, RESULTS OF SOIL WASHING TESTS FORSCHUYLKILL SITE

Water

Weight, g

No. 10No. 60PanFilter

Pb concentration

Wash filtrateNo. 10No. 60Fines

A

225.6369.4338.4210.9

, mg/kg

0.251,1703,1102,790

B

220.2359.2338.5174.6

for solids,

0.39615

1,2103,108

Surfactant

A

175.1348.3387.1133.6

mg/L for

36.61,2702,3002,310

B

161.6361.8377.1138.7

liquids

40.21,8901,2102,980

EDTA

A

119.5369.0440.1143.1

65.2422

3,2503,230

B

-4, " •

3E16C.,

81.81,3501,4304,760

TABLE C-4. RESULTS OF SOIL WASHING TESTS FORGOULD SOIL

Water

Weight, g

No. 10No. 60PanFilter

Pb concentration

Wash filtrateNo. 10No. 60Fines

A

231.3776.9136.769.2

» mg/kg

0.8133,20015,10036,400

B

209.3645.6135.270.1

for solids,

0.8229,50010,50046,400

Surfactant

A

149.5839.2121.646.5

mg/L for

12843,50014,30049,300

B

139.6846.3137.452.8

liquids

1257,7207,620

110,000

EDTA

A

145.1833.6 .142.969.9

3127,9609,13016,800

B

168.9818.3U4.7117.6

3359,9708,21013,700

C-4

$8302691

TABLE C-5. RESULTS OF SOIL WASHING TESTS FORGOULD CASINGS

Water Surfactant EDTA

Weight, g .__.._.__--_No. 10 .-561.7 533.4 367.1 471.4 403.2 523.3Pan 385.7 394.7 613,0 485.7 506.0 257.2Filter 258.9 .215.4 186.5 228.1 115.8 108.6

Pb concentration, mg/kg for solids, mg/L for liquids

Wash filtrate 1.17 1.46 394 373 81.3 185No. 10 64,100 7,300 9,880 78,700 17,700 67,300Fines .: 54,300 221,000 103,000 110,000 112,000 121,000

C-5

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